Ethanol → 3-Aminomethyl-4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazole ditosylate

HRID 963024

反応式

HRID 963024 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([CH2:18][CH3:19])[S:17][C:13]=2[N:12]2[C:20]([CH3:23])=[N:21][N:22]=[C:11]2[CH2:10][N:9]=1.C([OH:26])C.O.[C:28]1([CH3:38])[CH:33]=[CH:32][C:31]([S:34]([OH:37])(=[O:36])=[O:35])=[CH:30][CH:29]=1>O>[C:28]1([CH3:38])[CH:29]=[CH:30][C:31]([S:34]([OH:37])(=[O:35])=[O:36])=[CH:32][CH:33]=1.[C:28]1([CH3:38])[CH:29]=[CH:30][C:31]([S:34]([OH:37])(=[O:35])=[O:36])=[CH:32][CH:33]=1.[NH2:9][CH2:10][C:11]1[N:12]([C:13]2[S:17][C:16]([CH2:18][CH3:19])=[CH:15][C:14]=2[C:8](=[O:26])[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])[C:20]([CH3:23])=[N:21][N:22]=1

参加物

5

反応物 3

HCID 702EthanolHCID 3307EtizolamHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 190850953-Aminomethyl-4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazole ditosylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

4-(2-Chlorophenyl)-2-ethyl-9-methyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a] [1,4]diazepine (702 g) was suspended in a mixed solvent (4.9 l) of ethanol and water (9:1), and p-toluenesulfonic acid monohydrate (1165 g) was added. The mixture was stirred at 80° C. for 1.5 hours. The mixture was concentrated to about 2.5 l by evaporating the solvent under reduced pressure, and ethyl acetate (4 l) was added. The reaction mixture was filtered to give crystals, and the crystals were washed with ethyl acetate and ethanol and dried to give 1214 g of 3-aminomethyl-4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazole di-p-toluenesulfonate.

後処理

  1. additionwas added
  2. concentrationThe mixture was concentrated to about 2.5 l
  3. customby evaporating the solvent under reduced pressure, and ethyl acetate (4 l)
  4. additionwas added
  5. filtrationThe reaction mixture was filtered
  6. customto give crystals
  7. washthe crystals were washed with ethyl acetate and ethanol
  8. customdried

出典と根拠

ORDレコード
ord-c8e5dd973f9a439a90192d3c37e328c6
出典データセット
uspto-grants-1998_06
特許番号
US05760032

関連ノート

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