Potassium Carbonate → 8-Nitro-2H-benzo[B][1,4]oxazin-3(4H)-one

HRID 576072노트

반응식

HRID 576072 반응식
C(=O)([O-])[O-].[K+].[K+].Cl[CH2:8][C:9]([NH:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[C:13]=1[OH:21])=[O:10]>CN(C)C=O.C(OCC)(=O)C>[N+:18]([C:14]1[C:13]2[O:21][CH2:8][C:9](=[O:10])[NH:11][C:12]=2[CH:17]=[CH:16][CH:15]=1)([O-:20])=[O:19]

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 136462502-chloro-N-(2-hydroxy-3-nitrophenyl)acetamide

생성물 1

HCID 389971848-Nitro-2H-benzo[B][1,4]oxazin-3(4H)-one

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Potassium carbonate (4.10 g, 29.7 mmol) was added to a solution of 2-chloro-N-(2-hydroxy-3-nitrophenyl)acetamide obtained (5.70 g, 24.7 mmol) in N,N-dimethylformamide (150 mL) while cooling in ice, and the mixture was stirred at room temperature for 5 hr. The mixture was diluted with ethyl acetate, washed with water and brine, and then dried over anhydrous sodium sulfate. The desiccant was filtered off, followed by concentration under reduced pressure. The resulting residue was powdered with chloroform and collected by filtration to afford 8-nitro-2 H-1,4-benzoxazin-3(4 H)-one as a pale orange powder (4.32 g).

후처리

  1. temperaturewhile cooling in ice
  2. washwashed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationThe desiccant was filtered off
  5. concentrationfollowed by concentration under reduced pressure
  6. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-8a1bb5b27220403b85e7bccd8087180a
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09035059B2

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