Nitric Acid → 4-acetyl-3,4-dihydro-2,2-dimethyl-7-nitro-6-trifluoroacetylamino-2H-1,4-benzoxazine

HRID 1197772ノート

反応式

HRID 1197772 の反応式
[C:1]([N:4]1[C:9]2[CH:10]=[C:11]([NH:14][C:15](=[O:20])[C:16]([F:19])([F:18])[F:17])[CH:12]=[CH:13][C:8]=2[O:7][C:6]([CH3:22])([CH3:21])[CH2:5]1)(=[O:3])[CH3:2].[N+:23]([O-])([OH:25])=[O:24]>C(O)(=O)C>[C:1]([N:4]1[C:9]2[CH:10]=[C:11]([NH:14][C:15](=[O:20])[C:16]([F:18])([F:19])[F:17])[C:12]([N+:23]([O-:25])=[O:24])=[CH:13][C:8]=2[O:7][C:6]([CH3:22])([CH3:21])[CH2:5]1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 191048184-acetyl-3,4-dihydro-2,2-dimethyl-6-trifluoroacetylamino-2H-1,4-benzoxazine

生成物 1

HCID 191048224-acetyl-3,4-dihydro-2,2-dimethyl-7-nitro-6-trifluoroacetylamino-2H-1,4-benzoxazine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a solution of 22.0 g 4-acetyl-3,4-dihydro-2,2-dimethyl-6-trifluoroacetylamino-2H-1,4-benzoxazine in 100 ml acetic acid, was added dropwise a solution of 3.7 ml fuming nitric acid in 50 ml acetic acid, and the resulting solution was stirred at room temperature for two hours. The reaction mixture was poured into 600 ml ice water, the crystals which separated out were collected by filtration, and recrystallized from 100 ml ethanol, giving 21.6 g of 4-acetyl-3,4-dihydro-2,2-dimethyl-7-nitro-6-trifluoroacetylamino-2H-1,4-benzoxazine.

後処理

  1. customthe crystals which separated out
  2. filtrationwere collected by filtration
  3. customrecrystallized from 100 ml ethanol

出典と根拠

ORDレコード
ord-6525a8214b3e4536b0078c707bfd67ee
出典データセット
uspto-grants-1994_01
特許番号
US05278158

反応ノート

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