Carbon Tetrachloride → 1,1',1''-(Chlorosilylidyne)tris(benzene)

HRID 1940362

반응식

HRID 1940362 반응식
[Cr:1]([O:24][Si:25]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([O:4][Si:5]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)(=[O:3])=[O:2].C=C.C1([Si](C2C=CC=CC=2)(C2C=CC=CC=2)O)C=CC=CC=1.[O-2].[O-2].[O-2].[Cr+6].C1([Si](O[Si](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:110]>C(O)(=O)C.C(#N)C.C(C#N)CC>[C:6]1([Si:5]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[Cl:110])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cr:1]([O:24][Si:25]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)([C:38]1[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1)[C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)([O:4][Si:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)(=[O:3])=[O:2]

참가 물질

11

반응물 6

HCID 5943Carbon TetrachlorideHCID 6325EthyleneHCID 69925Triphenylsilanol4회HCID 74587Disiloxane, 1,1,1,3,3,3-hexaphenyl-HCID 10219390chromium (VI) trioxide3회HCID 178526121HCID 178526121, 화합물4회

생성물 2

HCID 64581,1',1''-(Chlorosilylidyne)tris(benzene)HCID 178526121HCID 178526121, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 6342Acetonitrile용매HCID 8008Butyronitrile용매

실험 절차

Bistriphenylsilyl chromate is usually used as the catalyst of unsaturated hydrocarbon compound polymerization such as ethylene polymerization. With respect to its synthesis process, early in 1958, U.S. Pat. 7,863,891 disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of 85% by reacting triphenylsilanol and chromium trioxide in glacial acetic acid at 50° C. for 10 minutes. L. M. Bakert et al disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of about 60% by reacting triphenylsilanol and chromium trioxide in carbon tetrachloride at room temperature for 24 hours [J. Org. Chem., Vol. 85, No. 8, pp. 774-776, March 1970]. The former Czechoslovakia Patent CS 175856 disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of 43-71% by reacting triphenylsilanol or triphenylsilyl ether and chromium trioxide in acetonitrile or propyl cyanide. However, the starting material triphenylsilanol used in the above processes is obtained by the hydrolysis of triphenylchlorosilane, so the process for the preparation of bistriphenylsilyl chromate is relatively complicated and the yield thereof is relatively low. The former Soviet Union Patent SU 689192 .disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of 94% by reacting triphenylchlorosilane and potassium dichromate in glacial acetic acid at 40°-50° C. for 1.5 hours. The reaction equation thereof is as follows: ##STR1##

후처리

  1. customWith respect to its synthesis process
  2. customcan be obtained with a yield of 85%
  3. customat 50° C.
  4. customfor 10 minutes
  5. customcan be obtained with a yield of about 60%
  6. customat room temperature
  7. customfor 24 hours
  8. customcan be obtained with a yield of 43-71%

출처 및 근거

ORD 기록
ord-8970a1da8b70416caac798b0fa5410c7
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05698723

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