Chlorosulfonic acid → 4-Ethoxy-3-(6-methyl-4-oxo-8-propyl-3,4-dihydro-imidazo[1,5-a][1,3,5]triazin-2-yl)-benzene-sulfonyl chloride

HRID 8621

反応式

HRID 8621 の反応式
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[NH:15][C:14](=[O:16])[N:13]2[C:17]([CH3:23])=[N:18][C:19]([CH2:20][CH2:21][CH3:22])=[C:12]2[N:11]=1)[CH3:2].[Cl:24][S:25](O)(=[O:27])=[O:26]>ClCCl>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([S:25]([Cl:24])(=[O:27])=[O:26])=[CH:6][C:5]=1[C:10]1[NH:15][C:14](=[O:16])[N:13]2[C:17]([CH3:23])=[N:18][C:19]([CH2:20][CH2:21][CH3:22])=[C:12]2[N:11]=1)[CH3:2]

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 1354758792-(2-ethoxyphenyl)-6-methyl-8-propyl-3H-imidazo[1,5-a][1,3,5]triazin-4-one

生成物 1

HCID 1354246684-Ethoxy-3-(6-methyl-4-oxo-8-propyl-3,4-dihydro-imidazo[1,5-a][1,3,5]triazin-2-yl)-benzene-sulfonyl chloride収率 99%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.64 g (5.25 mmol) of 2-(2-ethoxyphenyl)-6-methyl-8-propyl-3H-imidazo[1,5-a][1,3,5]triazin-4-one (example VI) are added in portions to 3.14 ml of chlorosulfonic acid while cooling with ice. The reaction mixture is stirred at room temperature for 16 hours, then diluted with dichloromethane and poured onto ice water. The organic phase is washed with water and dried over magnesium sulfate and the solvent is removed in vacuo. 2.15 g (99%) of 4-ethoxy-3-(6-methyl-4-oxo-8-propyl-3,4-dihydro-imidazo[1,5-a][1,3,5]triazin-2-yl)-benzene-sulfonyl chloride are obtained.

後処理

  1. temperaturewhile cooling with ice
  2. additionpoured onto ice water
  3. washThe organic phase is washed with water
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-b0655c26605e4b4cb0926cd201146d73
出典データセット
uspto-grants-2006_08
特許番号
US07091203B2

関連ノート

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