N-methyl-2-pyrrolidone → 8-amino-1-{4-[(aminothio)peroxy]phenyl}-1H-benzo[g]indazole-3-carboxamide

HRID 22980

반응식

HRID 22980 반응식
[NH2:1][C:2]1[CH:27]=[CH:26][C:5]2[CH2:6][CH2:7][C:8]3[C:9]([C:23]([NH2:25])=[O:24])=[N:10][N:11]([C:13]4[CH:18]=[CH:17][C:16]([O:19][O:20][S:21][NH2:22])=[CH:15][CH:14]=4)[C:12]=3[C:4]=2[CH:3]=1.CN1C(=O)CCC1>C1(C(C)C)C=CC=CC=1.[Pd]>[NH2:1][C:2]1[CH:27]=[CH:26][C:5]2=[CH:6][CH:7]=[C:8]3[C:12]([N:11]([C:13]4[CH:18]=[CH:17][C:16]([O:19][O:20][S:21][NH2:22])=[CH:15][CH:14]=4)[N:10]=[C:9]3[C:23]([NH2:25])=[O:24])=[C:4]2[CH:3]=1

참가 물질

5

반응물 2

HCID 13387N-methyl-2-pyrrolidoneHCID 222915508-amino-1-{4-[(aminothio)peroxy]phenyl}-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide

생성물 1

HCID 225925248-amino-1-{4-[(aminothio)peroxy]phenyl}-1H-benzo[g]indazole-3-carboxamide수율 90.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 7406Cumene용매

실험 절차

The product of Example 4b (1 g) and 5% Pd/C (300 mg) suspended in cumene (50 mL) and NMP (5 mL) was heated at reflux for 16 h. The mixture was then filtered and concentrated. The residue was diluted with methanol (10 mL) and added to water, after 1 h the resulting precipitate was collected by filtration and dried to yield the title compound (0.9 g).

후처리

  1. temperatureat reflux for 16 h
  2. filtrationThe mixture was then filtered
  3. concentrationconcentrated
  4. additionThe residue was diluted with methanol (10 mL)
  5. additionadded to water, after 1 h the resulting precipitate
  6. filtrationwas collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-8fce33b15a5c4c0e9f5294a5695d02da
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849653B2

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