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Potassium bisulfate → Ethyl 2-(mercaptomethyl)-1,4-dithiaspiro[4.4]nonane-7-acetate

HRID 1608271
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반응식

HRID 1608271 반응식
C([S:4][CH2:5][CH:6]1[CH2:10][S:9][C:8]2([CH2:14][CH2:13][CH:12]([CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:11]2)[S:7]1)(=O)C.[O-]CC.[Na+].OS([O-])(=O)=O.[K+]>C(O)C>[SH:4][CH2:5][CH:6]1[CH2:10][S:9][C:8]2([CH2:14][CH2:13][CH:12]([CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:11]2)[S:7]1
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참가 물질

5

반응물 3

HCID 516920Potassium bisulfateHCID 2723922Sodium ethoxideHCID 19849041Ethyl 2-[(acetylthio)methyl]-1,4-dithiaspiro[4.4]nonane-7-acetate

생성물 1

HCID 19849025Ethyl 2-(mercaptomethyl)-1,4-dithiaspiro[4.4]nonane-7-acetate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of the product of Example F and sodium ethoxide (prepared from 350 mg of sodium metal) in absolute ethanol (40 ml) was stirred for 1 hr under nitrogen. The reaction mixture was poured into 200 ml of 0.5N KHSO4 and extracted with ethyl acetate. After drying the organic phase over sodium sulfate, the solvent was removed on the rotary evaporator and the residue was chromatographed on silica gel using 5% ethyl acetate/hexane to give 2.1 g of the titled compound.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialAfter drying the organic phase over sodium sulfate
  3. customthe solvent was removed on the rotary evaporator
  4. customthe residue was chromatographed on silica gel using 5% ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-fb6a974e800d4575a8cbbc0854a4e0e6
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870098

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