Ethyl orthoformate → 4-n-Propyl-2,6,7-trithiabicyclo[2.2.2]octane
반응식
[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]참가 물질
4
실험 절차
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°).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-6f226eda447f4b4ca2c0a26702c6c37b
- 출처 데이터셋
- uspto-grants-1991_06
- 특허 번호
- US05026874
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