Hydroxyamine hydrochloride → 6-Amino-1-cyclopropyl-3,3-dimethyl-1H-pyrrolo[3,2-c]pyridin-2(3H)-one

HRID 1507606노트

반응식

HRID 1507606 반응식
[CH:1]1([N:4]2[C:12]3[CH:11]=[C:10]([N:13]=C(C4C=CC=CC=4)C4C=CC=CC=4)[N:9]=[CH:8][C:7]=3[C:6]([CH3:28])([CH3:27])[C:5]2=[O:29])[CH2:3][CH2:2]1.C([O-])(=O)C.[Na+].Cl.NO>CO>[NH2:13][C:10]1[N:9]=[CH:8][C:7]2[C:6]([CH3:28])([CH3:27])[C:5](=[O:29])[N:4]([CH:1]3[CH2:2][CH2:3]3)[C:12]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 900475681-Cyclopropyl-6-(diphenylmethyleneamino)-3,3-dimethyl-1H-pyrrolo[3,2-c]pyridin-2(3H)-one

생성물 1

HCID 900475166-Amino-1-cyclopropyl-3,3-dimethyl-1H-pyrrolo[3,2-c]pyridin-2(3H)-one

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
50 °C

실험 절차

A suspension of 1-cyclopropyl-6-(diphenylmethyleneamino)-3,3-dimethyl-1H-pyrrolo[3,2-c]pyridin-2(3H)-one (2.31 g, 6.06 mmol), sodium acetate (1.49 g, 18.2 mmol) and hydroxylamine hydrochloride (926 mg, 13.3 mmol) in methanol (60 ml) was heated to 50° C. for 3 hours. The reaction mixture was diluted with methanol, silica gel was added and the solvent was evaporated. The crude material was purified by flash chromatography on silica gel using dichloromethane/methanol as eluent. The title compound was obtained as off-white crystals (1.1 g).

후처리

  1. additionwas added
  2. customthe solvent was evaporated
  3. customThe crude material was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-b091d6ca87c74efbb8f8645b4f1922e5
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221816B2

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