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Ammonium Hydroxide → 2-(3-Mercapto-1-oxopropyl)-5-oxo-3-pyrazolidinecarboxylic acid

HRID 27261
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반응식

HRID 27261 반응식
C([S:4][CH2:5][CH2:6][C:7]([N:9]1[CH:13]([C:14]([OH:16])=[O:15])[CH2:12][C:11](=[O:17])[NH:10]1)=[O:8])(=O)C.[OH-].[NH4+]>>[SH:4][CH2:5][CH2:6][C:7]([N:9]1[CH:13]([C:14]([OH:16])=[O:15])[CH2:12][C:11](=[O:17])[NH:10]1)=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 14923Ammonium HydroxideHCID 23344444HCID 23344444, 화합물

생성물 1

HCID 233444412-(3-Mercapto-1-oxopropyl)-5-oxo-3-pyrazolidinecarboxylic acid수율 44.7%

실험 절차

DL-2-[3-(Acetylthio)-1-oxopropyl]-5-oxo-3-pyrazolidinecarboxylic acid (1.2 g) is treated in an argon atmosphere with 8 ml of a cold solution of 6.5 N ammonium hydroxide. After one hour at room temperature, the solution is extracted with ethyl acetate and treated with concentrated hydrochloric acid to pH 2. The water soluble product is extracted with five 20 ml portions of ethyl acetate. The combined extracts are dried over magnesium sulfate and evaporated to an oil which gradually solidifies. This material is dried in vacuo at 100° C. for 1 hour yielding 0.45 g of the title compound, melting point 140°-142° C.

후처리

  1. extractionthe solution is extracted with ethyl acetate
  2. addition
treated with concentrated hydrochloric acid to pH 2
  • extractionThe water soluble product is extracted with five 20 ml portions of ethyl acetate
  • dry with materialThe combined extracts are dried over magnesium sulfate
  • customevaporated to an oil which
  • customThis material is dried in vacuo at 100° C. for 1 hour
  • 출처 및 근거

    ORD 기록
    ord-39f6373776314ee2a372f4309ef8097e
    출처 데이터셋
    uspto-grants-1980_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04220791

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