反应详情

A mixture of methyl 7-benzenesulfonylamino-2,3-dihydro-1H-pyrrolo[1,2-a]indole-8-carboxylate (Intermediate 26, 0.075 g) and lithium hydroxide mononhydrate (0.049 g) in dioxane (2 mL) and water (1 mL) was irradiated in the microwave at 110° C. for 20 minutes. After cooling, the mixture was diluted with water and acidified to pH4-5 with formic acid. The resultant solid was washed with water and ether, then dried to give a cream powder. The solid was dissolved in methanol and acetone and freeze-dried, then dried in a dessicator, in vacuo, at 40° C. overnight. The solid was triturated with DCM and filtered, washed with DCM (1 mL) and pentane (1 mL) then dried in a dessicator, in vacuo, at 40° C. overnight. The yellow solid was dissolved in hot ethyl acetate and pentane was added until the mixture went cloudy. On cooling, the solid was collected by filtration, washed with pentane and dried in a dessicator, in vacuo, at 40° C. overnight to give 7-benzenesulfonylamino-2,3-dihydro-1H-pyrrolo[1,2-a]indole (0.023 g) as a cream solid.

1. temperatureAfter cooling
2. washThe resultant solid was washed with water and ether
3. customdried
4. customto give a cream powder
5. dry with materialacetone and freeze-dried
6. customdried in a dessicator, in vacuo, at 40° C. overnight
7. customThe solid was triturated with DCM
8. filtrationfiltered
9. washwashed with DCM (1 mL) and pentane (1 mL)
10. customthen dried in a dessicator, in vacuo, at 40° C. overnight
11. dissolutionThe yellow solid was dissolved in hot ethyl acetate
12. additionpentane was added until the mixture
13. temperatureOn cooling
14. filtrationthe solid was collected by filtration
15. washwashed with pentane
16. customdried in a dessicator, in vacuo, at 40° C. overnight