Ethyl orthoformate → 4-n-Propyl-2,6,7-trithiabicyclo[2.2.2]octane
反応式
[SH:1][CH2:2][C:3]([CH2:8][CH2:9][CH3:10])([CH2:6][SH:7])[CH2:4][SH:5].[CH:11](OCC)(OCC)OCC>C1C=CC=CC=1>[CH2:8]([C:3]12[CH2:6][S:7][CH:11]([S:5][CH2:4]1)[S:1][CH2:2]2)[CH2:9][CH3:10]参加物
4
実験手順
2-Mercaptomethyl-2-n-propylpropan-1,3-dithiol (4.0 g.) and triethyl orthoformate (3.6 g.) were refluxed, with stirring, in dry benzene (120 ml.) containing Amberlyst "15" (1.0 g.). The mixture was cooled and filtered. The filtrates were evaporated in vacuo and the residue was purified by chromatography on alumina eluting with 1:10, dichloromethane: hexane saturated with ammonia. 4-n-Propyl-2,6,7-trithiabicyclo[2.2.2]octane was obtained as a colourless solid (3.1 g., m.pt. 139°).
後処理
- additioncontaining Amberlyst "15" (1.0 g.)
- temperatureThe mixture was cooled
- filtrationfiltered
- customThe filtrates were evaporated in vacuo
- customthe residue was purified by chromatography on alumina eluting with 1:10, dichloromethane
出典と根拠
- ORDレコード
- ord-6f226eda447f4b4ca2c0a26702c6c37b
- 出典データセット
- uspto-grants-1991_06
- 特許番号
- US05026874
反応ノート
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