Hydrazine hydrate (1:1) → HCID 178451811、化合物

HRID 1888207ノート

反応式

HRID 1888207 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:24]#[N:25])[C:5](F)=[C:6]([C:8]([CH:10]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]2)=O)[CH:7]=1.O.[NH2:27][NH2:28]>C(O)C>[Br:1][C:2]1[CH:7]=[C:6]2[C:5](=[C:4]([C:24]#[N:25])[CH:3]=1)[NH:28][N:27]=[C:8]2[CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 59022871HCID 59022871、化合物

生成物 1

HCID 178451811HCID 178451811、化合物収率 59%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1,1-dimethylethyl 4-[(5-bromo-3-cyano-2-fluorophenyl)carbonyl]-1-piperidinecarboxylate (1.35 g, 3.3 mmols) and hydrazine hydrate (0.21 ml, 6.9 mmols) in ethanol (30 mL) was heated at reflux overnight. After cooling, the solvent was evaporated and the residue was purified by flash chromatography eluting with pentane/ethyl acetate 4:1 v/v to give the title compound (0.78 g) as a yellow solid (59%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. temperatureAfter cooling
  4. customthe solvent was evaporated
  5. customthe residue was purified by flash chromatography
  6. washeluting with pentane/ethyl acetate 4:1 v/v

出典と根拠

ORDレコード
ord-df771e4b77904824b85a5327e4120681
出典データセット
uspto-grants-2013_08
特許番号
US08501780B2

反応ノート

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