反应详情

温度

0 °C

Aluminum chloride (65.7 mg) was added in portions to tetrahydrofuran (5 mL) at 0° C. Under stirring a 10% solution of lithium aluminum hydride in tetrahydrofuran (1.35 mL) was slowly added while keeping the temperature below 10° C. The mixture was cooled to 0° C. and stirred for 15 minutes. A solution of trans-5-chloro-2,3,3a,12b-tetrahydro-2-methyl-1H-dibenz[2,3:6,7]oxepino[4,5-c]pyrrol-1-one (VII) (0.40 grams) in tetrahydrofuran (4 mL) was added to the mixture while keeping the temperature below 15° C. Stirring was continued for 2 hours at 10° C., whereupon 0.5 N sodium tartrate solution (15 mL) was added while keeping the temperature below 10° C. Stirring was continued for 15 minutes at 20° C. The salt layer was extracted twice with a toluene:ethyl acetate (8:2) mixture (25 mL).The combined organic layers were dried on magnesium sulphate, filtered and evaporated in vacuo to yield 0.36 grams (94%) of trans-5-chloro-2,3,3a,12b-tetrahydro-2-methyl-1H-dibenz[2,3:6,7]oxepino[4,5-c]pyrrole (A).

1. additionwas slowly added
2. customthe temperature below 10° C
3. customthe temperature below 15° C
4. stirringStirring
5. additionwas added
6. customthe temperature below 10° C
7. stirringStirring
8. waitwas continued for 15 minutes at 20° C
9. extractionThe salt layer was extracted twice with a toluene:ethyl acetate (8:2) mixture (25 mL).The combined organic layers
10. customwere dried on magnesium sulphate
11. filtrationfiltered
12. customevaporated in vacuo