참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 2-chloro-N,N-dimethylacetamide | HCID 75886 | — |
| 반응물 | methyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-amino-1-isopropenyl-5a,5b,8,8,11a-pentamethyl-2,3,3a,4,5,5a,5b,6,7,7a,8,11,11a,11b,12,13,13a,13b-octadecahydro-1H-cyclopenta[a]chrysen-9-yl)benzoate | HCID 68357865 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 86676594 | HCID 86676594 | 52% |
반응 단계
A mixture of methyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-amino-5a,5b,8,8,11a-pentamethyl-1-(prop-1-en-2-yl)-2,3,3a,4,5,5a,5b,6,7,7a,8,11,11a,11b,12,13,13a,13b-octadecahydro-1H-cyclopenta[a]chrysen-9-yl)benzoate (50 mg, 0.092 mmol), 2-chloro-N,N-dimethylacetamide (33.5 mg, 0.276 mmol), potassium phosphate (78 mg, 0.368 mmol) and potassium iodide (36.6 mg, 0.221 mmol) in acetonitrile (1 mL) was heated at 120° C. for 33 h in a sealed tube. The reaction mixture was quenched with distilled water (5 mL) and extracted with DCM (3×5 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the title compound as a pale yellow solid (30 mg, 52%). LCMS: m/e 629.51 (M+H)+, 3.03 min (method 10). The product was used in the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08846647B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-44529002305547538c8c62289208e1c4 |
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| 출처 메모 | uspto-grants-2014_09 |
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