Thionyl Chloride → HCID 178509690, 화합물

HRID 35918

반응식

HRID 35918 반응식
O[C:2]1([CH:9]([C:15]2[CH:22]=[CH:21][C:18]([C:19]#[N:20])=[CH:17][CH:16]=2)[C:10]2[N:14]=[CH:13][NH:12][N:11]=2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.S(Cl)(Cl)=O>ClCCl>[C:2]1(=[C:9]([C:15]2[CH:22]=[CH:21][C:18]([C:19]#[N:20])=[CH:17][CH:16]=2)[C:10]2[N:14]=[CH:13][NH:12][N:11]=2)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 178509720HCID 178509720, 화합물

생성물 1

HCID 178509690HCID 178509690, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

7 g of crude 4-[1-hydroxycyclohept-1-yl-1(1,2,4-triazolyl)methyl]benzonitrile is dissolved in 50 ml of dichloromethane at 0° and stirred with 20 ml of thionyl chloride for 1 hour at 0°. Then the mixture is concentrated to dryness under an oil pump vacuum, dissolved in 50 ml of dichloromethane, stirred for 2 hours with 30 ml of triethylamine, diluted with water, extracted three times with ethyl acetate, washed with sodium chloride solution, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, thus producing 1.9 g of 4-di-cycloheptylidene-1-(1,2,4triazolyl)methyl]benzonitrile as the free base, mp 79°-80°.

후처리

  1. concentrationThen the mixture is concentrated to dryness under an oil pump vacuum
  2. dissolutiondissolved in 50 ml of dichloromethane
  3. additiondiluted with water
  4. extractionextracted three times with ethyl acetate
  5. washwashed with sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated to dryness under vacuum
  8. customchromatographed on silica gel with hexane/ethyl acetate
  9. customthus producing 1.9 g of 4-di-cycloheptylidene-1-(1,2,4triazolyl)methyl]benzonitrile as the free base, mp 79°-80°

출처 및 근거

ORD 기록
ord-e12fcec478b04c62baf5bd535e7bea4a
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05411982

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