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Water → 7-hydroxyimino-7H-indolizino[5,6,7-ij]isoquinoline

HRID 267982
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반응식

HRID 267982 반응식
[CH:1]1[C:10]2[N:11]3[C:15]([C:16](=O)[C:8]4[C:9]=2[C:4]([CH:5]=[CH:6][N:7]=4)=[CH:3][CH:2]=1)=[CH:14][CH:13]=[CH:12]3.Cl.[NH2:19][OH:20].O>N1C=CC=CC=1>[OH:20][N:19]=[C:16]1[C:8]2[C:9]3[C:4]([CH:5]=[CH:6][N:7]=2)=[CH:3][CH:2]=[CH:1][C:10]=3[N:11]2[C:15]1=[CH:14][CH:13]=[CH:12]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 443297Hydroxyamine hydrochlorideHCID 215528757H-indolizino[5,6,7-ij]isoquinolin-7-one

생성물 1

HCID 1363535147-hydroxyimino-7H-indolizino[5,6,7-ij]isoquinoline수율 90.9%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 7H-indolizino[5,6,7-ij]isoquinolin-7-one (28 g.) and hydroxylamine hydrochloride (28 g.) in pyridine (560 cc.) is maintained at the boiling point, with stirring. The brown solution thus obtained is poured into water (3.92 liters). After stirring for 3 hours, the mustard yellow crystals obtained are filtered off and then washed copiously with water. After drying, 7-hydroxyimino-7H-indolizino[5,6,7-ij]isoquinoline (27.2 g.), melting at 254° C. with decomposition, is obtained. After recrystallisation from a mixture of water and pyridine (6- 5 by volume), the pure product melts at 258° C. with decomposition.

후처리

  1. customThe brown solution thus obtained
  2. stirringAfter stirring for 3 hours
  3. customthe mustard yellow crystals obtained
  4. filtrationare filtered off
  5. washwashed copiously with water
  6. customAfter drying

출처 및 근거

ORD 기록
ord-d46f2a13818c499691fb0d3e26646312
출처 데이터셋
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03946019

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