참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methyl Acrylate | HCID 7294 | — |
| 반응물 | Ethyl aluminium dichloride | HCID 16686341 | — |
| 반응물 | (3R,5R,8S,10S,13S,14S,Z)-17-Ethylidene-10,13-dimethyl-2,3,4,5,6,7,8,10,12,13,14,15,16,17-tetradecahydro-1H-cyclopenta[A]phenanthren-3-YL acetate | HCID 25145012 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Deoxycholic Acid Impurity 69 | HCID 25145010 | 70% |
반응 단계
Ethyl aluminum dichloride (14.2 mL, 25 mmol, 1.8M in toluene) was added to a solution of methyl acrylate (1.89 mL, 20 mmol) in DCM (60 mL) at 0° C. under inert atmosphere. The resulting solution was stirred for 15 min and then compound 1.6a (3 g, 8.7 mmol) was added. After stirring for an additional 20 min at 0° C., the temperature was raised to 25° C. and held there for a further 18 h. At this point the reaction was determined to be complete by TLC, then the mixture was poured into cold (0° C.) water (60 mL). The phases were separated and the aqueous layer was extracted with DCM (60 mL). The organic layers were combined and washed sequentially with water (50 mL) and saturated brine solution (100 mL). It was then dried over anhydrous Na2SO4 (5 g) and filtered. The filtrate was concentrated under vacuum, providing compound 1.7b (2.6 g, 70%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08367852B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_02 |
|---|
| ORD ID | ord-d8599c6ea62646a68e31b403b82a6062 |
|---|
| 출처 메모 | uspto-grants-2013_02 |
|---|
