1H-1,2,4-Triazole → HCID 54529319, 화합물

HRID 1980522노트

반응식

HRID 1980522 반응식
[H-].[Na+].[NH:3]1[CH:7]=[N:6][CH:5]=[N:4]1.[F:8][C:9]1[CH:14]=[CH:13][C:12]([Si:15]([C:20]2[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=2)([CH:17](Cl)[CH3:18])[CH3:16])=[CH:11][CH:10]=1.FC1C=CC([Si](C2C=CC(F)=CC=2)(CCCl)C)=CC=1>CN(C)C=O.O.ClCCl.CO>[F:26][C:23]1[CH:24]=[CH:25][C:20]([Si:15]([C:12]2[CH:11]=[CH:10][C:9]([F:8])=[CH:14][CH:13]=2)([CH3:16])[CH:17]([N:3]2[CH:7]=[N:6][CH:5]=[N:4]2)[CH3:18])=[CH:21][CH:22]=1

참가 물질

9

반응물 4

HCID 92571H-1,2,4-TriazoleHCID 24758Sodium hydrideHCID 20401745HCID 20401745, 화합물HCID 20401762HCID 20401762, 화합물

생성물 1

HCID 54529319HCID 54529319, 화합물수율 12%

시약·촉매·용매 4

HCID 887Methanol용매HCID 962Water용매HCID 6228Dimethylformamide용매2회HCID 6344Dichloromethane용매2회

실험 절차

A mixture of 1.78 g (37 mmol) of 50% sodium hydride, 30 ml of dimethylformamide, and 2.56 g (37 mmol) of 1H-1,2,4-triazole was stirred at 50° for one hour, and a solution of 10 g (33.7 mmol) of a 1:1 mixture of bis(4-fluorophenyl)-1-chloroethyl(methyl)silane and bis(4-fluorophenyl)-2-chloroethyl(methyl)silane in 10 ml of dimethylformamide was added. The mixture 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 sodium sulfate, and evaporated to leave a viscous oil. Chromatography over silica gel eluting with dichloromethane followed by 3% methanol in dichloromethane provided 1.37 g (12%) of the title compound as a viscous oil: nmr (CDCl3) 0.7 (3H, s), 1.6 (3H, d, J=7 Hz), 4.5 (1H, q, J=7 Hz), 6.9-7.7 (8H, m), 7.9 (1H, s), and 8.0 (1H, s).

후처리

  1. additionwas added
  2. stirringThe mixture was stirred at 50° for 64 hours
  3. temperaturecooled
  4. extractionextracted with ether
  5. washThe ether extracts were washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated
  8. customto leave a viscous oil

출처 및 근거

ORD 기록
ord-8503518506be4bdaaaa37734ef390892
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04510136

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