Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Imidazole → 1-Benzyl-3-t-butyldimethylsilyloxymethylpyrrolidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Imidazole | HCID 795 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 반응물 | (1-Benzylpyrrolidin-3-yl)methanol | HCID 5176654 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-Benzyl-3-t-butyldimethylsilyloxymethylpyrrolidine | HCID 19914927 | 86.7% |
반응 단계
Imidazole (30.0 g) was added to a solution of 1-benzyl-3-hydroxymethylpyrrolidine (43.45 g) and t-butyldimethylsilyl chloride (48.5 g) in dimethylformamide(150 ml) under ice-cooling. The mixture was stirred at the same temperature for 2 hours and at ambient temperature for 15 hours. The mixture was poured into water (600 ml), extracted twice with ethyl acetate (200 ml and 100 ml), dried over magnesium sulfate and evaporated under reduced pressure to give a syrup. The syrup was subjected to a column chromatography on silica gel (500 g) and eluted with a mixture of methanol and dichloromethane (5:95 V/V) to give 1-benzyl-3-t-butyldimethylsilyloxymethylpyrrolidine (60.15 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04923857 |
| 출처 데이터셋 | uspto-grants-1990_05 |
| ORD ID | ord-b1b110a41d2545c9b1e7640b3290c306 |
| 출처 메모 | uspto-grants-1990_05 |