Hydrazine hydrate (1:1) → HCID 178514446、化合物

HRID 1255452ノート

反応式

HRID 1255452 の反応式
C([O:3][C:4]([C@H:6]1[CH2:11][CH2:10][C@H:9]([OH:12])[CH2:8][CH2:7]1)=O)C.O.[NH2:14][NH2:15]>>[OH:12][C@H:9]1[CH2:10][CH2:11][C@H:6]([C:4]([NH:14][NH2:15])=[O:3])[CH2:7][CH2:8]1

参加物

3

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 178472487HCID 178472487、化合物

生成物 1

HCID 178514446HCID 178514446、化合物収率 91%

実験手順

A mixture of cis/trans-4-hydroxycyclohexane carboxylic acid ethyl ester (5.0 g, 29 mmol) and hydrazine hydrate (1.4 g, 29 mmol) was heated at reflux for 24 h. Residual water was removed by azeotropic distillation with toluene. The residue was triturated from tert-butyl methyl ether. The precipitate was collected by filtration and dried in vacuo to give the title compound as white solid in 91% yield.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 24 h
  3. customResidual water was removed by azeotropic distillation with toluene
  4. customThe residue was triturated from tert-butyl methyl ether
  5. filtrationThe precipitate was collected by filtration
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-2fa5d87c486649419bd1b8d562d726e2
出典データセット
uspto-grants-2013_06
特許番号
US08461151B2

反応ノート

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