Acetic Acid → HCID 563387、化合物

HRID 68538ノート

反応式

HRID 68538 の反応式
C([O:3][C:4]([NH:6][C:7](=[O:19])[C:8]([C:17]#[N:18])=[N:9][NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=O)C.C([O-])(=O)C.[Na+].C(O)(=O)C>O>[C:11]1([N:10]2[C:4](=[O:3])[NH:6][C:7](=[O:19])[C:8]([C:17]#[N:18])=[N:9]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 2822520Ethyl[2-cyano-2-(2-phenylhydrazono)acetamido]formate

生成物 1

HCID 563387HCID 563387、化合物収率 70%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

Intermediate b (21 g, 0.08 mol) and anhydrous sodium acetate (29 g, 0.35 mol) were added to glacial acetic acid (20v/w, 420 mL). The mixture was warmed up to react under reflux for 2 h. After completion of the reaction, the reaction solution was cooled to 0° C. and poured into water (1200 mL). The mixture was stirred for 30 min and filtered by suction. The filtered cake was washed with water and petroleum ether, and dried to produce an orange red solid (12 g) in a yield of 67.8%.

後処理

  1. temperatureThe mixture was warmed up
  2. customto react
  3. temperatureunder reflux for 2 h
  4. customAfter completion of the reaction
  5. filtrationfiltered by suction
  6. washThe filtered cake was washed with water and petroleum ether
  7. customdried

出典と根拠

ORDレコード
ord-105a12909b6245179ca0ecfa4091af6a
出典データセット
uspto-grants-2014_09
特許番号
US08822465B2

反応ノート

読み込み中…