Method for combined production of pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene and pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene

FIELD: chemistry.

SUBSTANCE: invention relates to a method for combined production of pentacyclo[7.5.0.02.8.05.14.07.11]tetradeca-3,12-diene of formula

and pentacyclo[8.4.0.03.7.04.14.06.11]tetradeca-8,12-diene of formula

The method includes homogenisation of 1,3,5-cycloheptatriene (CHT) in the presence of a Ti-containing catalyst system, and is characterised by that the catalyst used is Ti(acac)2Cl2-Et2AlCl, the reaction is carried out with molar ratio CHT:Ti(acac)2Cl2:Et2AlCl=10:(0.1-0.3):4, in an argon atmosphere, at 5-80°C, in benzene for 6-72 hours.

EFFECT: method enables to use a more stable catalyst and reduces power consumption.

1 tbl, 7 ex

 

The invention relates to methods of producing new polycyclic compounds, specifically to a method of producing pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene of formula (1) and pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene of the formula (2)

These compounds belong to the class of intense energy consuming systems and may find application as components of high-energy fuels for air-breathing missile systems (G. W. Burdette, H. R. Lander, J. R. McCoy, J. Energy, 1978, 2, 289), intermediates in the synthesis of practically important derivatives of adamantane and diamantane used to obtain an effective antiviral and antiparkinsonian drugs (F. Turecek, V. Hanus, P. Sedmera, H. Antropiusova, K. Mach, Coll. "To Czechoslovak Chem. Commun, 1981, 46, 1474).

The known method [K. Mach, H. Antropiusova, F. Turecek, V. Hanus, P. Sedmera. Zwei neue pentacyclische dimere des cycloheptatriens // Tetrahedron Lett, 1980, V. 21, 4879] receiving pentacyclic dimers (1) and (2) reaction of homodimerization 1,3,5-cycloheptatriene (CHT) in the presence of a catalyst TiCl4-Et2AlCl at a temperature of 40°C for 6 hours in a total yield of 40% according to the scheme

A new method of synthesis pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene (1) and pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene(2).

<> The method consists in homodimerization CGT in the presence of a catalytic system Ti(acac)2Cl2-Et2AlCl, taken in the molar ratio CGT:Ti(acac)2Cl2:Et2AlCl=10:(0.1-0.3):4, preferably 10:0.2:4. The reaction is carried out in an argon atmosphere at a temperature of 5-80°C. the reaction Time occurs 6-72 h, the total output of homodimeric 76-98% in the ratio(1):(2)=1:2. As a solvent it is necessary to use benzene.

The reaction proceeds according to the scheme

Target products (1) and (2) are formed only with the participation of CGT and catalytic system Ti(acac)2Cl2-Et2AlCl. In the presence of other transition metal complexes (for example, Cp2ZrCl2, Cp2TiCl2, Zr(acac)4, Pd(acac)2, Fe(ASAS)3) target products (1) and (2) are not formed.

Conducting the reaction in the presence of a catalyst Ti(acac)2Cl2more than 0.3 mmol to 10 mmol CGT does not significantly increase the yield of target products (1) and (2). The use in the reaction of the catalyst Ti(acac)2Cl2less than 0.1 mmol to 10 mmol CGT reduces the output gameaddict (1) and (2), which is associated with a reduction of catalytically active sites in the reaction mass. The experiments were performed at heating 5-80°C. At a higher temperature (e.g. 80°C) decreases the output of homodimers, probably due to a side p�of acesso decomposition and polymerization. At a lower temperature (e.g. 20°C) decreases the reaction rate.

Significant differences of the proposed method:

1. The proposed method is based on the use of the catalytic system Ti(acac)2Cl2-Et2AlCl, allowing to obtain homodimer (1) and (2) in a total yield of 97% (in the ratio(1):(2)=1:2). In the conventional method homodimer (1) and (2) obtained using the catalytic system of TiCl4-Et2AlCl in a total yield of 40% in the ratio(1):(2)=9:1.

The proposed method has the following advantages:

1. The method allows to obtain high yields of homodimer (1) and (2). In addition, the catalyst based on bis-acetylacetonate of titjikala [Ti(acac)2Cl2] is the most preferred because it has a number of advantages compared with TiCl4due to their high stability, crystallinity and 100% reproducible results, which greatly simplifies its use for preparative purposes.

2. The use of bis-acetylacetonate of titjikala [Ti(acac)2Cl2] in the reaction of homodimerization 1,3,5-cycloheptatriene can significantly reduce power consumption for the target homodimers by lowering the reaction temperature to 5°C in contrast to the known method (40°C)

The method is illustrated by the following examples.

EXAMPLE 1. In a glass reactor in an atmosphere of dry ar�it under stirring downloaded 1 g (10 mmol) of 1,3,5-cycloheptatriene, 0.063 g (0.2 mmol) of Ti(acac)2Cl2, 4 ml of dry benzene and was loaded with 0.6 ml (4 mmol, 90.2%) Et2AlCl in 1 ml of benzene. The mixture was stirred at 40°C for 6 h. the reaction mixture was treated with 7-10% HCl solution. Get pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene (1) and pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene (2) in a total yield of 97%.

Spectral characteristics of homodimers (1) and (2):

The NMR spectrum1H (CDCl3d, M. D.) 7-pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene (1): 1.68-1.75 (m, 2H, C(6)H2,); 1.82-1.98 (m, 1H, C(11)H); 2.51-2.57 (m, 1H, C(7)H); 2.73-3.00 (m, 7H, C(1,5,8,9,14)H, C(10)H2); 3.21 (1H, C(2)H, J=9 Hz); 5.27 (t, 1H, C(13)H, J=10 Hz); 5.56 (t, 1H, C(4)H, J=10 Hz); 6.03 (t, 1H, C(12)H, J=10 Hz); 6.24 (t, 1H, C(3)H, J=10 Hz).

The NMR spectrum13C (CDCl3d, M. D.) 7-pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene (1): 31.43 (C(6)); 35.18 (C(11)); is at 39.48 (C(2)); 40.16 (C(14)); 40.22 (C(10)); 40.57 (C(9)); 50.12 (C(7)); 53.22 (C(8)); 127.78 (C(13)); 128.28 (C(4)); 133.53 (C(12)); 139.59 (C(3)).

The NMR spectrum1H (CDCl3d, M. D.) pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene (2): 1.11-1.16 (m, 2H, C(2,5) (H2,); 1.28 (d, 2H, C(2,5) (H2, J=12 Hz); 1.80-1.81 (m, 2H, C(1,6) (H); 1.99 (t, 2H, C(10,11)H, J=7 Hz); 2.24-2.26 (m, 2H, C(3,4) (H); 2.60 (2H, C(7,14)H, J=8 Hz); 5.90 (t, 2H, C(13,8)H, J=8 Hz); 6.08 (t, 2H, C(9,12)H, J=8 Hz).

The NMR spectrum13C (CDCl3d, M. D.) pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene (2): 31.63 (C(2,5)); 36.0 (C(1,6)); 38.67 (C(10,11)); 40.14 (C(3,4)); 43.33 (C(7,14)); 128.96 (C(13,8)); 132.33 (C(9,12)). Other examples of the method are shown in table 1.

Table 1
№ p/pThe molar ratio CGT:Ti(ASAS)2Cl2:Et2AlCl, mmolTemperature, °CReaction time, hThe ratio of (1) and (2)Total output (1) and (2), %
110:0.2:44061:297
210:0.2:48061:276
310:0.2:42081:298
410:0.2:45721:288
510:0.2:4 6061:296
610:0.1:44061:284
710:0.3:44061:299

A method for co-production pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene of formula (1) and pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene of the formula (2)

characterized by homodimerization 1,3,5-cycloheptatriene (CHT) in the presence of Ti-containing catalytic system, characterized in that as the catalyst, Ti(acac)2Cl2-Et2AlCl, the reaction is carried out at a molar ratio of CGT:Ti(acac)2Cl2:Et2AlCl=10:(0.1-0.3):4, in argon atmosphere, at 5-80°C, in benzene, for occurs 6-72 hours



 

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