Acetic Acid → 4-Bromo-3-methylbenzohydrazide

HRID 336369노트

반응식

HRID 336369 반응식
C(O)(=O)C.C(OC([NH:12][NH:13][C:14](=[O:23])[C:15]1[CH:20]=[CH:19][C:18]([Br:21])=[C:17]([CH3:22])[CH:16]=1)=O)(C)(C)C>ClCCl>[Br:21][C:18]1[CH:19]=[CH:20][C:15]([C:14]([NH:13][NH2:12])=[O:23])=[CH:16][C:17]=1[CH3:22]

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 86690170N'-(4-bromo-3-methyl-benzoyl)-hydrazinecarboxylic acid tert-butyl ester

생성물 1

HCID 39058874-Bromo-3-methylbenzohydrazide수율 51.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

500 mL trifluor acetic acid was added to 70 g N′-(4-bromo-3-methyl-benzoyl)-hydrazinecarboxylic acid tert-butyl ester in 1 L dichlormethane. The reaction was stirred 1 h at RT and evaporated. The residue was basicfied with 1N sodiumhydroxide and extracted with saturated sodiumchloride solution and tetrahyrofuran. The organic layer was evaporated and the residue crystallized with ethyl acetate to give 25 g desired product.

후처리

  1. customevaporated
  2. extractionextracted with saturated sodiumchloride solution and tetrahyrofuran
  3. customThe organic layer was evaporated
  4. customthe residue crystallized with ethyl acetate

출처 및 근거

ORD 기록
ord-125d8aeb8e25486aa41a4b26d6d0b998
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889677B2

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