beta-(p-Chlorophenyl)-alpha-methylene-gamma-butyrolactone → S-[[4-(4-chlorophenyl)-2-oxooxolan-3-yl]methyl] benzenecarbothioate

HRID 65261노트

반응식

HRID 65261 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][O:12][C:10](=[O:11])[C:9]2=[CH2:14])=[CH:4][CH:3]=1.[C:15]([OH:23])(=[S:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C1(C)C=CC=CC=1.C(N(CC)CC)C.C(OCC)C>[C:15]([S:22][CH2:14][CH:9]1[CH:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[CH2:13][O:12][C:10]1=[O:11])(=[O:23])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

6

반응물 2

HCID 20234200beta-(p-Chlorophenyl)-alpha-methylene-gamma-butyrolactoneHCID 178526132HCID 178526132, 화합물

생성물 1

HCID 13715528S-[[4-(4-chlorophenyl)-2-oxooxolan-3-yl]methyl] benzenecarbothioate수율 75%

시약·촉매·용매 3

HCID 8471Triethylamine촉매HCID 1140Toluene용매HCID 3283Diethyl Ether용매

실험 절차

To a solution of 600 mg of β-(p-chlorophenyl)-α-methylene-γ-butyrolactone in 10 ml of toluene were added 0.44 ml of thiobenzoic acid and one drop of triethylamine and the reaction was effected at room temperature for 18 hours. The reaction mixture was diluted with 100 ml of ethyl ether, washed with water and saturated saline, dried over magnesium sulfate and the solvent was then distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 750 mg (yield 75%) of the title compound.

후처리

  1. washwashed with water and saturated saline
  2. dry with materialdried over magnesium sulfate
  3. distillationthe solvent was then distilled off
  4. customThe crude product thus obtained
  5. customwas purified by a silica gel column chromatography

출처 및 근거

ORD 기록
ord-3b7073b3151c4a99bac17ba77a9f95d0
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613613

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