Acetic Acid → 4-Fluoro-3-methylbenzohydrazide

HRID 239181ノート

反応式

HRID 239181 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]([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]

参加物

4

反応物 2

HCID 176Acetic AcidHCID 86686514N'-(4-Fluoro-3-methyl-benzoyl)-hydrazinecarboxylic acid tert-butyl ester

生成物 1

HCID 632093974-Fluoro-3-methylbenzohydrazide収率 83.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fba27b8f0c1c4370a96ed3d7253a19d1
出典データセット
uspto-grants-2014_02
特許番号
US08642774B2

反応ノート

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