反应详情

5-(1-benzyl-pyrrolidin-3-yloxy)-2-methyl-1H-indole-3-carboxylic acid benzyl ester (0.118 g, 0.268 mmol, 1.0 eq.) was dissolved in dry 1,2-dichloroethane (5 mL) and treated with α-chloroethyl chloroformate (0.035 mL, 0.32 mmol, 1.2 eq.). The reaction was heated to reflux and followed by TLC (hexane/ethyl acetate 1/1). After 2 hours, the reaction was concentrated in vacuo, redissolved in methanol (5 mL), and heated to reflux. After 4 hours, the crude hydrochloride salt was precipitated from methanol/ethyl acetate/hexane to afford a brown solid, which was carried directly to the next step.

1. temperatureThe reaction was heated
2. temperatureto reflux
3. concentrationthe reaction was concentrated in vacuo
4. dissolutionredissolved in methanol (5 mL)
5. temperatureheated to reflux
6. waitAfter 4 hours
7. customthe crude hydrochloride salt was precipitated from methanol/ethyl acetate/hexane
8. customto afford a brown solid, which