反应详情

To a vigorously stirred solution/suspension of the product from example 69 part f) (0.393 g) and solid sodium bicarbonate (0.342 g) in DCM (3 ml) and water (3 ml) was added benzenesulfonyl chloride (0.21 ml) dropwise. The mixture was stirred for 16 h. The organic layer and 1 further DCM extract were combined and purified by passage through SCX resin eluting with MeCN, MeOH followed by 7M NH3 in MeOH. The basic fractions were concentrated in vacuo, dissolved in DCM (3 ml) and treated with TFA (20 ml) for 16 h. Concentration in vacuo and purification by RPHPLC gave the title product as a white foam (45 mg).

1. extractionThe organic layer and 1 further DCM extract
2. custompurified by passage through SCX resin
3. washeluting with MeCN, MeOH
4. concentrationThe basic fractions were concentrated in vacuo
5. dissolutiondissolved in DCM (3 ml)
6. additiontreated with TFA (20 ml) for 16 h
7. concentrationConcentration
8. customin vacuo and purification by RPHPLC