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

HRID 576072ノート

反応式

HRID 576072 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8a1bb5b27220403b85e7bccd8087180a
出典データセット
uspto-grants-2015_05
特許番号
US09035059B2

反応ノート

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