反应详情

A mixture of 7.75 ml. of methanesulfonyl chloride in 200 ml. of toluene is added, over a period of one hour, to a stirred mixture of 21.2 g. of benzoin, 28 ml. of triethylamine and 100 ml. of toluene. The mixture is allowed to stand 2 hours, 100 ml. of water is added and the emulsion is filtered giving a solid which is washed with water and dried, giving 14.5 g. of benzoin methanesulfonate esters. A 2.90 g. portion of benzoin methanesulfonate esters and 1.30 g. of hexahydro-2H-1,3-diazepin-2-thione are suspended in 50 ml. of warm acetone and heated at reflux for 4 hours. The mixture is cooled, the solid is collected, washed with acetone then ether and dried in vacuo at 60° C., giving 3.9 g. of the desired product, m.p. 176°-178° C.

1. additionA mixture of 7.75 ml
2. filtrationthe emulsion is filtered
3. customgiving a solid which
4. washis washed with water
5. customdried
6. customgiving 14.5 g
7. temperatureat reflux for 4 hours
8. temperatureThe mixture is cooled
9. customthe solid is collected
10. washwashed with acetone
11. dry with materialether and dried in vacuo at 60° C.
12. customgiving 3.9 g