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

HRID 22980

反応式

HRID 22980 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 7406Cumene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8fce33b15a5c4c0e9f5294a5695d02da
出典データセット
uspto-grants-2005_02
特許番号
US06849653B2

関連ノート

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