Potassium Hydroxide → alpha-Cyclohexylthiomethyl-beta-(p-methoxyphenyl)-gamma-butyrolactone

HRID 65264

반응식

HRID 65264 반응식
[OH-].[K+].CS(O[CH2:8][CH:9]1[CH:14]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=2)[CH2:13][O:12][C:10]1=[O:11])(=O)=O.[CH:23]1([SH:29])[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1>C(O)C.C(OCC)C>[CH:23]1([S:29][CH2:8][CH:9]2[CH:14]([C:15]3[CH:16]=[CH:17][C:18]([O:21][CH3:22])=[CH:19][CH:20]=3)[CH2:13][O:12][C:10]2=[O:11])[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 15290CyclohexanethiolHCID 20234197alpha-Methanesulfonyloxymethyl-beta-(p-methoxyphenyl)-gamma-butyrolactone

생성물 1

HCID 13518978alpha-Cyclohexylthiomethyl-beta-(p-methoxyphenyl)-gamma-butyrolactone수율 22%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

To a solution of 480 mg of potassium hydroxide in 40 ml of ethanol were added 2.0 g of α-methanesulfonyloxymethyl-β-(p-methoxyphenyl)-γ-butyrolactone and 1.6 ml of cyclohexylmercaptan and the resulting mixture was kept at room temperature for 4 hours. After completion of the reaction, the reaction mixture was diluted with 200 ml of ethyl ether, washed with water and saturated saline, dried over magnesium sulfate and the solvent was distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 600 mg (yield 22%) of the title compound.

후처리

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

출처 및 근거

ORD 기록
ord-ba41b964acd849fab487151f8f23f48f
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613613

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