Sulfuric Acid → 5-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide

HRID 487247

반응식

HRID 487247 반응식
S(=O)(=O)(O)[OH:2].[CH:6]1([N:11]2[C:15]([NH2:16])=[C:14]([C:17]#[N:18])[C:13]([CH2:19][CH3:20])=[N:12]2)[CH2:10][CH2:9][CH2:8][CH2:7]1>[OH-].[NH4+]>[CH:6]1([N:11]2[C:15]([NH2:16])=[C:14]([C:17]([NH2:18])=[O:2])[C:13]([CH2:19][CH3:20])=[N:12]2)[CH2:7][CH2:8][CH2:9][CH2:10]1

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 158712691-cyclopentyl-3-ethyl-4-cyano-5-amino-1H-pyrazole

생성물 1

HCID 224493525-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide수율 85%

시약·촉매·용매 1

HCID 14923Ammonium Hydroxide용매

실험 절차

To concentrated sulfuric acid (50 ml) cooled in an ice/sodium chloride bath was added in small portions 1-cyclopentyl-3-ethyl-4-cyano-5-amino-1H-pyrazole. The reaction mixture was warmed to room temperature and stirred for 24 hours. The reaction mixture was slowly added to a solution of concentrated ammonium hydroxide (150 ml) in ice-water (500 ml). A yellow precipitate formed which was collected by filtration, washed with water and dried at 90° C. for 60 hours in high vacuum to afford 3.47 g (85%) of 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide, m.p. 167°-168° C.

후처리

  1. customA yellow precipitate formed which
  2. filtrationwas collected by filtration
  3. washwashed with water
  4. customdried at 90° C. for 60 hours in high vacuum

출처 및 근거

ORD 기록
ord-db7ff469404f431ba334272effe88955
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294612

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