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

HRID 576073ノート

反応式

HRID 576073 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-186321116b2e44dc91fadf96bd7afeb6
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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