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Butyl chloroformate → 2-Amino-1-n-butoxycarbonyl-4,5-dicyanoimidazole

HRID 1576950
ノート
印刷プレビュー

反応式

HRID 1576950 の反応式
[NH2:1][C:2]1[NH:3][C:4]([C:9]#[N:10])=[C:5]([C:7]#[N:8])[N:6]=1.C(=O)(O)[O-].[Na+].Cl[C:17]([O:19][CH2:20][CH2:21][CH2:22][CH3:23])=[O:18]>CC(C)=O>[NH2:1][C:2]1[N:3]([C:17]([O:19][CH2:20][CH2:21][CH2:22][CH3:23])=[O:18])[C:4]([C:9]#[N:10])=[C:5]([C:7]#[N:8])[N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 61140Butyl chloroformateHCID 1704461H-Imidazole-4,5-dicarbonitrile, 2-amino-HCID 516892Sodium Bicarbonate

生成物 1

HCID 102202732-Amino-1-n-butoxycarbonyl-4,5-dicyanoimidazole

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

2 g of 2-amino-4,5-dicyanoimidazole was dissolved in 20 ml of suspension of acetone containing 1.3 g of sodium bicarbonate and then 2.1 g of n-butyl chloroformate was added dropwise to said solution at a room temperature. The resulting solution was refluxed during 30 minutes, and white crystal was separated out when the rection mixture was poured into ice-water. After recrystallizing the crude product from methanol, 2.7 g of the purified compound having a melting point of 170° to 172°C was obtained as needles (Yield rate: 77%).

後処理

  1. customat a room temperature
  2. temperatureThe resulting solution was refluxed during 30 minutes
  3. customwhite crystal was separated out when the rection mixture
  4. additionwas poured into ice-water
  5. customAfter recrystallizing the crude product from methanol, 2.7 g of the purified compound
  6. customwas obtained as needles (Yield rate: 77%)

出典と根拠

ORDレコード
ord-74a95b4112994c06a0bccf0a4f944f1f
出典データセット
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03983241

反応ノート

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