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

HRID 633457노트

반응식

HRID 633457 반응식
[CH3:1][N:2]1[C:19](=[O:20])[N:5]2[C:6]3[CH:15]=[C:14]([N+:16]([O-])=O)[CH:13]=[CH:12][C:7]=3[O:8][C:9]([CH3:11])([CH3:10])[C:4]2=[N:3]1>CO.[Pd]>[NH2:16][C:14]1[CH:13]=[CH:12][C:7]2[O:8][C:9]([CH3:11])([CH3:10])[C:4]3[N:5]([C:19](=[O:20])[N:2]([CH3:1])[N:3]=3)[C:6]=2[CH:15]=1

참가 물질

4

반응물 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

생성물 1

HCID 867045448-amino-2,4,4-trimethyl-2,4-dihydro-1H-benzo[b][1,2,4]triazolo[4,3-d][1,4]oxazin-1-one수율 110.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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) and 10% Pd—C were suspended in methanol (5 mL). The reaction mixture was stirred at room temperature under H2 atmosphere (1 atm) overnight. The catalyst was filtered off over celite and washed with methanol (5×20 mL). The filtrate was evaporated to give 8-amino-2,4,4-trimethyl-2,4-dihydro-1H-benzo[b][1,2,4]triazolo[4,3-d][1,4]oxazin-1-one (245 mg, quant).

후처리

  1. filtrationThe catalyst was filtered off over celite
  2. washwashed with methanol (5×20 mL)
  3. customThe filtrate was evaporated

출처 및 근거

ORD 기록
ord-d901a16435ab443bbf96d5d141376198
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321763B2

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