Acetic Acid → 4-Bromo-3-methylbenzohydrazide

HRID 336369ノート

反応式

HRID 336369 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 39058874-Bromo-3-methylbenzohydrazide収率 51.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-125d8aeb8e25486aa41a4b26d6d0b998
出典データセット
uspto-grants-2014_11
特許番号
US08889677B2

反応ノート

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