Methanol → HCID 20401795, 화합물

HRID 1980523노트

반응식

HRID 1980523 반응식
[C:1]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][C:4]([Si:7]([CH3:12])([CH3:11])[CH:8](Cl)[CH3:9])=[CH:3][CH:2]=1.[K].[NH:20]1[CH:24]=[N:23][CH:22]=[N:21]1.CO>CN(C)C=O.O.ClCCl>[C:1]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][C:4]([Si:7]([CH3:12])([CH3:11])[CH:8]([N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)[CH3:9])=[CH:3][CH:2]=1

참가 물질

7

반응물 3

HCID 887MethanolHCID 20401742HCID 20401742, 화합물HCID 534465811,2,4-Triazole potassium

생성물 1

HCID 20401795HCID 20401795, 화합물수율 13.1%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 2.50 g (7.46 mmol) of 82% pure (1,1'-biphenyl-4-yl)dimethyl-1-chloroethylsilane and 1.60 g (15 mmol) of 1H-1,2,4-triazole potassium salt in 15 ml of dimethylformamide was stirred at 50° for 64 hours, cooled, diluted with water, and extracted with ether. The ether extracts were washed with water and brine, dried over magnesium sulfate, and evaporated to leave a viscous oil. Chromatography over silica gel eluting with 2% methanol in dichloromethane gave 0.30 g (13%) of the title compound as a pale yellow oil: nmr (CDCl3) 0.38 and 0.42 (total 6H, two equal s), 1.6 (3H, d, J=7 Hz), 4.2 (1H, q, J=7 Hz), 7.3-7.8 (9H, m), 7.9 (1H, s) and 8.0 (1H, s).

후처리

  1. temperaturecooled
  2. extractionextracted with ether
  3. washThe ether extracts were washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customto leave a viscous oil

출처 및 근거

ORD 기록
ord-01a983b83e2d4092b650d8a1804ac584
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04510136

반응 노트

불러오는 중…