Sulfuric Acid → 3-[2-(Dimethylamino)ethyl]-N-methyl-1H-indole-5-methanesulphonamide sulphate

HRID 724918

反応式

HRID 724918 の反応式
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[CH3:6][N:7]([CH3:25])[CH2:8][CH2:9][C:10]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([CH2:19][S:20]([NH:23][CH3:24])(=[O:22])=[O:21])[CH:17]=2)[NH:12][CH:11]=1>O.C(O)C>[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[CH3:25][N:7]([CH3:6])[CH2:8][CH2:9][C:10]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([CH2:19][S:20]([NH:23][CH3:24])(=[O:21])=[O:22])[CH:17]=2)[NH:12][CH:11]=1

参加物

5

反応物 2

HCID 1118Sulfuric AcidHCID 5358Sumatriptan

生成物 1

HCID 670562903-[2-(Dimethylamino)ethyl]-N-methyl-1H-indole-5-methanesulphonamide sulphate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

反応条件

温度
45 °C

実験手順

Sulphuric acid solution (2N,169 ml) was diluted with water (106 ml) and added rapidly dropwise to a stirred solution of 3-[2-(dimethylamino)ethyl]-N-methyl-1H-indole-5-methanesulphonamide (100 g) in ethanol (2.3 l) and water (25 ml) at reflux. The resulting solution was cooled to 45° C.; then seeded, cooled to 4° C. and aged 1 h. The reaction mixture was filtered and the filtrate washed with ethanol (50 ml) then dried at 40° C. in vacuo to give the title compound (114 g) in a solvated form, m.p. 157° C. (decomp.).

後処理

  1. temperatureat reflux
  2. temperaturecooled to 4° C. and aged 1 h
  3. filtrationThe reaction mixture was filtered
  4. washthe filtrate washed with ethanol (50 ml)
  5. customthen dried at 40° C. in vacuo

出典と根拠

ORDレコード
ord-a66ad6d2d69149a4ad04bb3e496dcb14
出典データセット
uspto-grants-1998_01
特許番号
US05705520

関連ノート

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