反应详情

A solution of (R)-5-hydroxy-5-(3-pyridyl)pentyl thioacetate (2.8 g) in dry dichloro- methane (15 ml) under a nitrogen atmosphere is cooled to -15° C. and treated with triethylamine (1.4 g) using a syringe. It is then treated with methanesulphonyl chloride (1.5 g) by syringe during 5 minutes. The temperature rises spontaneously to -8° C. during this addition. When the addition is complete the reaction mixture is allowed to warm to room temperature. After 2 hours it is washed with water (4×15 ml) until its pH is 7. The organic phase is then dried with magnesium sulphate, filtered and evaporated under reduced pressure, to give (R)-5-methanesulphonyloxy-5-(3-pyridyl)pentyl thioacetate (3.66 g), in the form of a yellow oil. This material is used in the next step without further purification.

1. additionThe temperature rises spontaneously to -8° C. during this addition
2. additionWhen the addition
3. washAfter 2 hours it is washed with water (4×15 ml) until its pH is 7
4. dry with materialThe organic phase is then dried with magnesium sulphate
5. filtrationfiltered
6. customevaporated under reduced pressure