Water → 2,4,4-trimethyl-8-nitro-2,4-dihydro-1H-benzo[b][1,2,4]triazolo[4,3-d][1,4]oxazin-1-one

HRID 633456ノート

反応式

HRID 633456 の反応式
[CH3:1][C:2]1([CH3:19])[O:7][C:6]2[CH:8]=[CH:9][C:10]([N+:12]([O-:14])=[O:13])=[CH:11][C:5]=2[N:4]2[C:15](=[O:18])[NH:16][N:17]=[C:3]12.I[CH3:21].[H-].[Na+].O>CN(C=O)C>[CH3:21][N:16]1[C:15](=[O:18])[N:4]2[C:5]3[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:6]=3[O:7][C:2]([CH3:19])([CH3:1])[C:3]2=[N:17]1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 867045424,4-dimethyl-8-nitro-2,4-dihydro-1H-benzo[b][1,2,4]triazolo[4,3-d][1,4]oxazin-1-one

生成物 1

HCID 867045432,4,4-trimethyl-8-nitro-2,4-dihydro-1H-benzo[b][1,2,4]triazolo[4,3-d][1,4]oxazin-1-one収率 92%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4,4-Dimethyl-8-nitro-2,4-dihydro-1H-benzo[b][1,2,4]triazolo[4,3-d][1,4]oxazin-1-one, iodomethane (73 μL, 1.2 eq.) were dissolved in DMF (4 mL). Sodium hydride (58 mg, 60% suspension in oil, 1.5 eq.) was added to the solution in an ice bath. The reaction mixture was stirred at room temperature for two hours. Water (15 mL) was added to the reaction. White precipitation was filtered and washed with water to give 2,4,4-trimethyl-8-nitro-2,4-dihydro-1H-benzo[b][1,2,4]triazolo[4,3-d][1,4]oxazin-1-one (249 mg, 92% yield in two steps).

後処理

  1. customWhite precipitation
  2. filtrationwas filtered
  3. washwashed with water

出典と根拠

ORDレコード
ord-a6be1222eeab4a81be6113d9e6a37228
出典データセット
uspto-grants-2016_04
特許番号
US09321763B2

反応ノート

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