Hydrochloric Acid → Scopine hydrochloride

温度

0 °C

10.0 g (22.84 mmol) of scopolamine hydrobromide trihydrate was suspended in 100 mL of absolute ethanol, and cooled to about 0° C. Sodium borohydride (4.0 g, 105.7 mmol) was then added portion-wise while maintaining the temperature at a maximum of 30° C.4.8 mL of water was then added to the reaction mixture. After 3.5 hours, the reaction was completed and 50 mL of diethyl ether was then added. The reaction was then cooled to 0° C., and acidified with 2M hydrochloric acid in diethyl ether to a pH of about 2. The suspension was stirred at room temperature for 30 minutes and then filtered on GochP3. The white solid was dried at 45° C. under vacuum for 4 hours, yielding 9 g of product containing 79% of salts determined by sulphuric ashes.

1. temperaturewhile maintaining the temperature at a maximum of 30° C
2. temperatureThe reaction was then cooled to 0° C.
3. filtrationfiltered on GochP3
4. customThe white solid was dried at 45° C. under vacuum for 4 hours

ORDレコード

ord-f9a99855698a4e72a2f02fc2f97dd071

出典データセット

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08344143B2