Hydrochloric Acid → HCID 22009947, 화합물

HRID 322091노트

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HRID 322091 반응식
[OH-].[Na+].[O:3]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]([C:28]3[C:36]4[C:31](=[CH:32][C:33]([C:37]([O:39]C)=[O:38])=[CH:34][CH:35]=4)[N:30]([CH3:41])[CH:29]=3)[C:13]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][C:20]=3[O:26][CH3:27])(=[O:18])=[O:17])=[O:14])=[CH:11][C:6]=2[O:5][CH2:4]1.Cl>CO.O.ClCCl>[O:3]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]([C:28]3[C:36]4[C:31](=[CH:32][C:33]([C:37]([OH:39])=[O:38])=[CH:34][CH:35]=4)[N:30]([CH3:41])[CH:29]=3)[C:13]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][C:20]=3[O:26][CH3:27])(=[O:17])=[O:18])=[O:14])=[CH:11][C:6]=2[O:5][CH2:4]1

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 224672003-{1-(1,3-Benzodioxol-5-yl)-2-[(2-methoxy-4-methylphenyl)sulfonamido]-2-oxoethyl}-6-(methoxycarbonyl)-1-methyl-1h-indole

생성물 1

HCID 22009947HCID 22009947, 화합물수율 92.4%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 6344Dichloromethane용매

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온도
45 °C

실험 절차

Aqueous sodium hydroxide (9.0 liters of a 20% aqueous solution) was added to a stirred suspension of methyl 3-{1-(1,3-benzodioxol-5-yl)-2-[(2-methoxy4-methylphenyl)-sulfonylamino]-2-oxoethyl}-1-methyl-1H-indole-6-carboxylate (from step (b), 5.0 kg) in methanol (25 liters) and demineralised water (20 liters). The suspension was warmed to 45° C. for 1.5 h, cooled to room temperature and diluted with dichloromethane (25 liters). The pH of the aqueous phase was adjusted to 3 with the addition of concentrated hydrochloric acid (7.0 liters) and the phases separated. The organic phase was concentrated to low volume and filtration of the precipitated product gave the subtitle compound as a white crystalline solid (4.5 kg, 92%).

후처리

  1. temperaturecooled to room temperature
  2. customthe phases separated
  3. concentrationThe organic phase was concentrated to low volume and filtration of the precipitated product

출처 및 근거

ORD 기록
ord-28c678a1082440e2872b6f2bf976e2a3
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211223B1

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