Acetic Acid → 4-Fluoro-3-methylbenzohydrazide

HRID 239181노트

반응식

HRID 239181 반응식
C(O)(=O)C.C(OC([NH:12][NH:13][C:14](=[O:23])[C:15]1[CH:20]=[CH:19][C:18]([F:21])=[C:17]([CH3:22])[CH:16]=1)=O)(C)(C)C>ClCCl>[F: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 86686514N'-(4-Fluoro-3-methyl-benzoyl)-hydrazinecarboxylic acid tert-butyl ester

생성물 1

HCID 632093974-Fluoro-3-methylbenzohydrazide수율 83.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

50 mL trifluor acetic acid was added to 13 g N′-(4-fluoro-3-methyl-benzoyl)-hydrazinecarboxylic acid tert-butyl ester in 150 mL dichlormethane. The reaction was stirred for 1 h at RT and the solvent was evaporated. The residue was basicfied with 1 N sodium hydroxide and extracted with saturated sodium chloride solution and tetrahydrofuran. The organic layer was evaporated and the residue crystallized from ethyl acetate to yield 6.8 g of the desired product.

후처리

  1. customthe solvent was evaporated
  2. extractionextracted with saturated sodium chloride solution and tetrahydrofuran
  3. customThe organic layer was evaporated
  4. customthe residue crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-fba27b8f0c1c4370a96ed3d7253a19d1
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642774B2

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