反応式
Cl.Cl.[CH3:3][NH:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[NH2:13].C([O-])(=O)C.[K+].[C:25](=S)=[S:26].C(S)(=S)N.[Cl-].[K+]>C(O)(C)C>[CH3:3][N:4]1[C:25](=[S:26])[NH:13][CH:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5]1参加物
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
To a suspension of 15 g (50 mmol) of 2-[(methylamino)methyl]-α-phenylbenzenemethanamine dihydrochloride in 100 mL of isopropyl alcohol was added 10 g (100 mmol) of potassium acetate followed by 3.3 mL (55 mmol) of carbon disulfide in 35 mL of isopropyl alcohol. The suspension was stirred at room temperature for one and one-half hours and then refluxed for 30 minutes. The reaction was chilled in ice and the internal salt of the carbamodithioic acid, contaminated with two equivalents of potassium chloride, was filtered off. The carbamodithioic acid was suspended in 125 mL of 95% ethanol, and 1.3 mL of 12N hydrochloric acid was added. The suspension was refluxed for three days, cooled, and 15.3 g (114%) of the crude benzodiazepin-3-thione was filtered off. A 6-g portion of the crude product was recrystallized from 2-ethoxy ethanol to yield 2.0 g (38%) of product, mp 208-209.
後処理
- temperaturerefluxed for 30 minutes
- temperatureThe reaction was chilled in ice
- filtrationwas filtered off
- addition1.3 mL of 12N hydrochloric acid was added
- temperatureThe suspension was refluxed for three days
- temperaturecooled
- filtration15.3 g (114%) of the crude benzodiazepin-3-thione was filtered off
- customA 6-g portion of the crude product was recrystallized from 2-ethoxy ethanol
出典と根拠
- ORDレコード
- ord-f0ac08a8be49426cafff99098869b47e
- 出典データセット
- uspto-grants-1995_01
- 特許番号
- US05380721
関連ノート
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