反应详情

Chlorosulphonic acid (18 mL) was added to a solution of the product from step (e) (32.3 g) in acetonitrile (100 ml) at least 9° C. When addition was complete, the mixture was warmed to room temperature. The resulting crystals were filtered off, washed with acetonitrile/pet. ether, dried, taken up in a mixture of 50% w/v aqu. KOH (100 mL) and water (55 mL) and distilled over KOH to give the desired product as a colourless oil (16.1 g). 1H NMR consistent with the proposed structure.

1. additionWhen addition
2. filtrationThe resulting crystals were filtered off
3. washwashed with acetonitrile/pet. ether
4. customdried
5. additiontaken up in a mixture of 50%
6. distillationKOH (100 mL) and water (55 mL) and distilled over KOH