Sodium Bicarbonate → (1R,3aS,5aR,5bR,7aR,11aR,11bR,13aR,13bR)-3a-amino-5a,5b,8,8,11a-pentamethyl-1-(prop-1-en-2-yl)octadecahydro-1H-cyclopenta[a]chrysen-9(5bH)-one

To a solution of (1R,3aS,5aR,5bR,7aR,11aR,11bR,13aR,13bR)-5a,5b,8,8,11a-pentamethyl-9-oxo-1-(prop-1-en-2-yl)icosahydro-1H-cyclopenta[a]chrysen-3a-aminium chloride (462 mg, 1.000 mmol) in DCM (6 mL) was added saturated solution of sodium bicarbonate 10 mL. The 2-phase mixture was vigorously stirred, DCM layer separated, it was washed with another portion of 6 mL of saturated sodium bicarbonate solution. The mixture was extracted with 10 mL DCM three times. The combine DCM fractions was finally washed with 5 mL DI water. Upon evaporation and drying, a thick semi-solid was isolated. This crude material was used in the next step without further purification.

1. customDCM layer separated
2. washit was washed with another portion of 6 mL of saturated sodium bicarbonate solution
3. extractionThe mixture was extracted with 10 mL DCM three times
4. washThe combine DCM fractions was finally washed with 5 mL DI water
5. customUpon evaporation
6. customdrying
7. customa thick semi-solid was isolated
8. customThis crude material was used in the next step without further purification

ORD 기록

ord-bd6bf5396f9b40f987436c826d1e4d02

출처 데이터셋

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08906889B2