反应详情

A solution of 95 (7.6 g, 0.025 mol) in pyridine (15 ml) was cooled in an ice bath and p-toluenesulfonyl chloride (4.7 g, 0.025 mol) was added while keeping the internal temperature below 30° C. After stirring for 3 hours at room temperature, a saturated solution of Na2CO3 was added and the mixture extracted with CH2Cl2 (3×). The organic extracts were dried, filtered and concentrated under reduced pressure below 50° C. initially using water aspirator pressure and finally high vacuum to yield the p-toluene sulfonate of 95 (0.025 mol).

1. customthe internal temperature below 30° C
2. extractionthe mixture extracted with CH2Cl2 (3×)
3. customThe organic extracts were dried
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure below 50° C. initially using water aspirator pressure and finally high vacuum