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Pyridine → 8-(Acetylamino)-1-{4-[(aminothio)peroxy]phenyl}-4,5-dihydro-1h-benzo[g]indazole-3-carboxamide

HRID 22981
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HRID 22981 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.[C:28](OC(=O)C)(=[O:30])[CH3:29].N1C=CC=CC=1>CN(C=O)C.O>[C:28]([NH: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:14]=[CH:15][C:16]([O:19][O:20][S:21][NH2:22])=[CH:17][CH:18]=4)[C:12]=3[C:4]=2[CH:3]=1)(=[O:30])[CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 222915508-amino-1-{4-[(aminothio)peroxy]phenyl}-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide

생성물 1

HCID 222918058-(Acetylamino)-1-{4-[(aminothio)peroxy]phenyl}-4,5-dihydro-1h-benzo[g]indazole-3-carboxamide수율 90%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매
2회

실험 절차

To the material of Example 4b (1.0 g, 0.0026 mol) in DMF (15 mL) was added dropwise a mixture of acetic anhydride (0.283 mL, 0.003 mol) and pyridine (0.243 mL, 0.003 mol) in DMF (5 mL). Contents were stirred overnight, diluted with water (75 mL), and filtered to give the desired as a white solid, 1.0 g (90% yield). FABHRMS m/z 426.1235 (M+H, C20H20N5O4S requires 426.1236). 1H NMR (DMSO-d6/300 MHz) 9.80 (s, 1H); 8.00 (d, 2H); 7.75 (d, 2H); 7.60 (s, 1H); 7.48 (s, 2H); 7.39 (s, 1H); 7.30 (d, 1H); 7.15 (s, 1H); 2.90 (s, 4H); 1.92 (s, 3H). Anal. Calcd for C20H19N5O4S (1H2O): C, 54.17; H, 4.77; N, 15.79. Found: C, 54.20; H, 4.97; N, 15.77.

후처리

  1. filtrationfiltered
  2. customto give the

출처 및 근거

ORD 기록
ord-c6fb776b7fb54d0488b78a408fa548fd
출처 데이터셋
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06849653B2

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