Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,2-Dimethoxypropane → 3-tert-Butyl 4-methyl 2,2-dimethyl-1,3-oxazolidine-3,4-dicarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 반응물 | Methyl N-(tert-butoxycarbonyl)serinate | HCID 495564 | — |
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-tert-Butyl 4-methyl 2,2-dimethyl-1,3-oxazolidine-3,4-dicarboxylate | HCID 5138497 | — |
반응 단계
To a solution of (34) in CH2Cl2, stirring under nitrogen at 0° C., was added 2,2-dimethoxypropane (29.5 mL, 237.9 mmol) and p-toluene sulfonic acid monohydrate (9.050 g, 47.58 mmol). The mixture was removed from the ice bath after 15 minutes and stirred at room temperature for 1.5 hours. The reaction mixture was poured into 50 mL of saturated NaHCO3 (aq) and extracted with diethyl ether (3×50). The organic layer was extracted with NaHCO3 and brine, then dried over anhydrous MgSO4, filtered and concentrated under reduced pressure. The crude material was purified by flash chromatography on SiO2 (1:1 EtOAc/Hexanes) to yield 7.659 g (62%, 3 steps) of a clear liquid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07560477B2 |
| 출처 데이터셋 | uspto-grants-2009_07 |
| ORD ID | ord-f4e26cbfd17f43a99a07407087df0fdf |
| 출처 메모 | uspto-grants-2009_07 |