Carbon Disulfide → Perhydrobenzimidazole-2-thione
反応式
[C:1](=[S:3])=S.[NH2:4][C@@H:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C@@H:6]1[NH2:11]>C(Cl)Cl>[NH:4]1[C@H:5]2[CH2:10][CH2:9][CH2:8][CH2:7][C@H:6]2[NH:11][C:1]1=[S:3]参加物
4
実験手順
A solution of carbon disulfide (1.1 mL, 17.9 mmol) and CH2Cl2 (10 mL) was treated dropwise with cis-1,2-diaminocyclohexane 20-1 (Aldrich) (2.0 g, 17.5 mmol) while maintaining the reaction mixture temperature below 20° C. with an ice bath. The reaction mixture was stirred at ambient temperature for 2.0 h after the addition was complete. Concentration followed by refluxing the resulting solid in H2O (20 mL) for 20 h gave a yellow solution. The cooled solution was extracted with CH2Cl2 and the CH2Cl2 portion was dried (MgSO4) and concentrated. The pale yellow solid was recrystallized from CH2Cl2 /ether to give 20-2 as a pale yellow solid. mp=164-166° C.
後処理
- temperaturewhile maintaining the reaction mixture temperature below 20° C. with an ice bath
- additionafter the addition
- concentrationConcentration
- temperatureby refluxing the resulting solid in H2O (20 mL) for 20 h
- customgave a yellow solution
- extractionThe cooled solution was extracted with CH2Cl2
- dry with materialthe CH2Cl2 portion was dried (MgSO4)
- concentrationconcentrated
- customThe pale yellow solid was recrystallized from CH2Cl2 /ether
出典と根拠
- ORDレコード
- ord-4ea14fb098a94fbfa362012e502f5820
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05929120
反応ノート
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