Water → 4-methyl-8-nitro-2H-1,4-benzoxazin-3(4H)-one

HRID 576073노트

반응식

HRID 576073 반응식
[H-].[Na+].[N+:3]([C:6]1[C:15]2[O:14][CH2:13][C:12](=[O:16])[NH:11][C:10]=2[CH:9]=[CH:8][CH:7]=1)([O-:5])=[O:4].[CH3:17]I.O>CN(C)C=O>[CH3:17][N:11]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([N+:3]([O-:5])=[O:4])[C:15]=2[O:14][CH2:13][C:12]1=[O:16]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 389971848-Nitro-2H-benzo[B][1,4]oxazin-3(4H)-one

생성물 1

HCID 389971764-methyl-8-nitro-2H-1,4-benzoxazin-3(4H)-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium hydride (60%) (300 mg, 7.50 mmol) was added to a solution of 8-nitro-2 H-1,4-benzoxazin-3(4 H)-one (971 mg, 5.00 mmol) in N,N-dimethylformamide (15 mL) at room temperature, the mixture was stirred for 10 min, and then methyl iodide (374 μL, 6.00 mmol) was added dropwise thereto. The mixture was stirred at room temperature for 3 hr and water was added to the reaction mixture. The resulting precipitate was collected by filtration, washed with ethyl acetate and water, and then dried at 60° C. under reduced pressure to afford 4-methyl-8-nitro-2 H-1,4-benzoxazin-3(4 H)-one as a pale yellow amorphous substance (453 mg).

후처리

  1. stirringThe mixture was stirred at room temperature for 3 hr
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with ethyl acetate and water
  4. customdried at 60° C. under reduced pressure

출처 및 근거

ORD 기록
ord-186321116b2e44dc91fadf96bd7afeb6
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09035059B2

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