참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Chlorotriethylsilane | HCID 13819 | — |
| 반응물 | 10-deacetylbaccatin III | HCID 154272 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | 7-O-(Triethylsilyl) Baccatin III | HCID 9939927 | 77% |
반응 단계
182 g of triethylsilyl chloride are added over 1 hour 20 minutes to a solution of 293.9 g of 10-deacetylbaccatin III in 2.7 liters of pyridine. The solution obtained is stirred for 40 hours at 5° C. 360 g of acetic anhydride are then added while the temperature is maintained at 5° C. The suspension obtained is stirred for 48 hours at 20° C. and then poured into 40 liters of ice-cold water. The precipitate obtained is separated by filtration, then washed with 8 times 2 liters of water and lastly dissolved in 3 liters of ethyl acetate. The organic phase is dried over magnesium sulphate. After filtration and concentration under reduced pressure, the product obtained is crystallized in isopropyl ether. 7-(Triethylsilyl)baccatin III is thereby obtained in a 77% yield, the characteristics of which product are as follows:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05959125 |
|---|
| 출처 데이터셋 | uspto-grants-1999_09 |
|---|
| ORD ID | ord-64b6443b641f4ba481be1bfbe1569598 |
|---|
| 출처 메모 | uspto-grants-1999_09 |
|---|