Ammonia → (+/-)-3-(2-Pyridyl)-4,5-dihydro-1-(3-mercapto-1-oxopropyl)-1H-pyrazole-5-carboxylic acid

HRID 127001노트

반응식

HRID 127001 반응식
N.C([S:5][CH2:6][CH2:7][C:8]([N:10]1[CH:14]([C:15]([OH:17])=[O:16])[CH2:13][C:12]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)=[N:11]1)=[O:9])(=O)C>>[N:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[C:12]1[CH2:13][CH:14]([C:15]([OH:17])=[O:16])[N:10]([C:8](=[O:9])[CH2:7][CH2:6][SH:5])[N:11]=1

참가 물질

3

반응물 2

HCID 222AmmoniaHCID 20288727(+/-)-1-[3-(Acetylthio)-1-oxopropyl]-3-(2-pyridyl)-4,5-dihydro-1H-pyrazole-5-carboxylic acid

생성물 1

HCID 20288735(+/-)-3-(2-Pyridyl)-4,5-dihydro-1-(3-mercapto-1-oxopropyl)-1H-pyrazole-5-carboxylic acid

실험 절차

Aqueous ammonia (12 ml of 7 N) is stirred at 0°-5° C. under argon and 3.5 g of (±)-1-[3-(acetylthio)-1-oxopropyl]-3-(2-pyridyl)-4,5-dihydro-1H-pyrazole-5-carboxylic acid is added. The resulting solution is stirred for 2 hours under argon and is then extracted with ethyl acetate (discarded). The aqueous layer is acidified with acetic acid and extracted with ethyl acetate (three 50 ml portions). The combined organic layers are washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to yield the title compound.

후처리

  1. extractionis then extracted with ethyl acetate (discarded)
  2. extractionextracted with ethyl acetate (three 50 ml portions)
  3. washThe combined organic layers are washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-71cc72670eb44bdeabe440da9b22a19b
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254267

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