Dichlorodiphenylsilane → HCID 4351769, 화합물

HRID 1906292

반응식

HRID 1906292 반응식
[CH2:1]([Mg]Br)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].Cl[Si:22](Cl)([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>>[CH2:1]([Si:22]([CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

참가 물질

3

반응물 2

HCID 6627Dichlorodiphenylsilane2회HCID 178442890HCID 178442890, 화합물

생성물 1

HCID 4351769HCID 4351769, 화합물수율 78%

실험 절차

The first portion of the octadecylmagnesium bromide was cooled to 0° and cuprous cyanide (0.12 g 1.34 mmoles) was added with stirring. Then dichlorodiphenylsilane (1.95 ml, 9.27 mmoles) was added. The reaction mixture was stirred at 10° for 140 minutes. Gas chromatographic analysis showed that most of the dichlorodiphenylsilane had disappeared during the first hour of reaction. The mixture was then stirred at room temperature for about 16 hours (i.e. overnight). The reaction mixture was then filtered, quenched with water, and acidified slightly with HCl. After extraction with diethylether, drying (with MgSO4) and removal of solvent, a solid was obtained. Extraction with hot heptane and crystallization provided 4.96 g of dioctadecyldiphenylsilane. The yield was about 78%.

후처리

  1. stirringThe reaction mixture was stirred at 10° for 140 minutes
  2. customhad disappeared during the first hour of reaction
  3. stirringThe mixture was then stirred at room temperature for about 16 hours (i.e. overnight)
  4. filtrationThe reaction mixture was then filtered
  5. customquenched with water
  6. extractionAfter extraction with diethylether
  7. customdrying
  8. custom(with MgSO4) and removal of solvent
  9. customa solid was obtained
  10. extractionExtraction
  11. customwith hot heptane and crystallization

출처 및 근거

ORD 기록
ord-965c22f5de6a4bfa9e31a0a5b952a12b
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04650891

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