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Hydroxyamine hydrochloride → HCID 136359213, 화합물

HRID 1156795
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반응식

HRID 1156795 반응식
[Cl:1][C:2]1[C:16]([Cl:17])=[C:15]([OH:18])[CH:14]=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=O.Cl.[NH2:20][OH:21]>N1C=CC=CC=1>[Cl:1][C:2]1[C:16]([Cl:17])=[C:15]([OH:18])[CH:14]=[CH:13][C:3]=1[C:4](=[N:20][OH:21])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 13015711HCID 13015711, 화합물

생성물 1

HCID 136359213HCID 136359213, 화합물수율 96%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 31.8 g (0.11 m) of 2,3-dichloro-4-hydroxy-2'-fluorobenzophenone of Example 2B and 15.29 g (0.22 m) of hydroxylamine hydrochloride in 150 ml of pyridine is refluxed 64 hours. The pyridine is evaporated in vacuo, 5% HCl added, extracted with ethyl acetate, dried (Na2SO4) and evaporated to give 32 g (96%) of 2,3-dichloro-4-hydroxy-2'-fluorobenzophenone oxime. An analytical sample is recrystallized from ethanol/H2O, m.p. 168°-175° C. TLC indicates the product is a mixture of isomers.

후처리

  1. customThe pyridine is evaporated in vacuo, 5% HCl
  2. additionadded
  3. extractionextracted with ethyl acetate
  4. dry with materialdried (Na2SO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-991f793faab846c297babf1bc7d82474
출처 데이터셋
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04337261

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