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

HRID 1197772노트

반응식

HRID 1197772 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-6525a8214b3e4536b0078c707bfd67ee
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05278158

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