Hydrochloric Acid → HCID 22009947、化合物

HRID 322091ノート

反応式

HRID 322091 の反応式
[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

参加物

7

反応物 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

生成物 1

HCID 22009947HCID 22009947、化合物収率 92.4%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
45 °C

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-28c678a1082440e2872b6f2bf976e2a3
出典データセット
uspto-grants-2001_04
特許番号
US06211223B1

反応ノート

読み込み中…