Methanol → 4-acetyl 6-amino-3,4-dihydro-2,2-dimethyl-7-nitro-2H-1,4-benzoxazine

HRID 1197773ノート

反応式

HRID 1197773 の反応式
[C:1]([N:4]1[C:9]2[CH:10]=[C:11]([NH:17]C(=O)C(F)(F)F)[C:12]([N+:14]([O-:16])=[O:15])=[CH:13][C:8]=2[O:7][C:6]([CH3:25])([CH3:24])[CH2:5]1)(=[O:3])[CH3:2].CO.C(=O)(O)[O-].[Na+]>O>[C:1]([N:4]1[C:9]2[CH:10]=[C:11]([NH2:17])[C:12]([N+:14]([O-:16])=[O:15])=[CH:13][C:8]=2[O:7][C:6]([CH3:25])([CH3:24])[CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 887MethanolHCID 516892Sodium BicarbonateHCID 191048224-acetyl-3,4-dihydro-2,2-dimethyl-7-nitro-6-trifluoroacetylamino-2H-1,4-benzoxazine

生成物 1

HCID 191048204-acetyl 6-amino-3,4-dihydro-2,2-dimethyl-7-nitro-2H-1,4-benzoxazine収率 85.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 21.6 g 4-acetyl-3,4-dihydro-2,2-dimethyl-7-nitro-6-trifluoroacetylamino-2H-1,4-benzoxazine, 500 ml methanol, 50 ml water and 10.5 g sodium bicarbonate was stirred at room temperature for seven hours, the reaction mixture was poured into 1.5 l ice water, and the precipitate which separated out was collected by filtration and recrystallized from 450 ml ethanol, giving 13.5 g of 4-acetyl-6-amino-3,4-dihydro-2,2-dimethyl-7-nitro-2H-1,4-benzoxazine.

後処理

  1. customthe precipitate which separated out
  2. filtrationwas collected by filtration
  3. customrecrystallized from 450 ml ethanol

出典と根拠

ORDレコード
ord-d9c1f5b2f1754a0d8280fa239f3dada8
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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