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 633456노트

반응식

HRID 633456 반응식
[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

참가 물질

6

반응물 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

생성물 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-one수율 92%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-a6be1222eeab4a81be6113d9e6a37228
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321763B2

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