Urea → 5-Amino-6-nitro-1H-isoindole-1,3(2H)-dione

HRID 920470

反応式

HRID 920470 の反応式
Cl[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:7](=[O:14])[NH:6][C:5]2=[O:15].[NH2:16]C(N)=O>O>[NH2:16][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:7](=[O:14])[NH:6][C:5]2=[O:15]

参加物

4

反応物 2

HCID 1176UreaHCID 28011294-Chloro-5-nitrophthalimide

生成物 1

HCID 151445685-Amino-6-nitro-1H-isoindole-1,3(2H)-dione収率 92.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A mixture of 5-chloro-6-nitroisoindoline-1,3-dione (28.0 g, 0.123 mol) and urea (73.8 g, 1.23 mol) was stirred and heated to 150° C. under argon for 6 h. After cooled to rt, the solid was suspended in hot water (100 mL, 80° C.), filtered, washed with hot water (3×50 mL) and dried under vacuum to give a yellow solid product, 23.56 g, 92.5% yield.

後処理

  1. temperatureAfter cooled to rt
  2. filtrationfiltered
  3. washwashed with hot water (3×50 mL)
  4. customdried under vacuum
  5. customto give a yellow solid product, 23.56 g, 92.5% yield

出典と根拠

ORDレコード
ord-ed47e73b7daf467f93712a427a8e6c1c
出典データセット
uspto-grants-2016_03
特許番号
US09273055B2

関連ノート

読み込み中…