Methoxyacetyl chloride → 3,5-Bis(methoxyacetylamino)-4-chlorobenzonitrile

HRID 1165880ノート

反応式

HRID 1165880 の反応式
[Cl:1][C:2]1[C:9]([NH2:10])=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[NH2:11].[CH3:12][O:13][CH2:14][C:15](Cl)=[O:16]>N1C=CC=CC=1>[CH3:12][O:13][CH2:14][C:15]([NH:11][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([NH:10][C:15](=[O:16])[CH2:14][O:13][CH3:12])[C:2]=1[Cl:1])[C:6]#[N:7])=[O:16]

参加物

4

反応物 2

HCID 96623Methoxyacetyl chlorideHCID 124029953,5-Diamino-4-chlorobenzonitrile

生成物 1

HCID 146992833,5-Bis(methoxyacetylamino)-4-chlorobenzonitrile

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 4-chloro-3,5-diaminobenzonitrile (3.34 g) in pyridine (60 ml) is added dropwise methoxyacetyl chloride (4.0 ml) at room temperature. The mixture is stirred at room temperature for 2 hours, and thereafter, pyridine is distilled off under reduced pressure. To the residue is added water, and the resulting solid substance is separated by filtration and washed with water. The resulting crude crystals are recrystallized from ethanol to give the title compound (5.1 g) having the following physical properties.

後処理

  1. distillationpyridine is distilled off under reduced pressure
  2. additionTo the residue is added water
  3. customthe resulting solid substance is separated by filtration
  4. washwashed with water
  5. customThe resulting crude crystals are recrystallized from ethanol

出典と根拠

ORDレコード
ord-012e51196b8f4431b52d32b3bb8cf243
出典データセット
uspto-grants-1990_03
特許番号
US04912135

反応ノート

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