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4-Methylmorpholine → 1-(t-Butyldimethylsilyloxy)-3-(p-nitrophenoxycarbonyloxy)propane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 4-Nitrophenyl chloroformate | HCID 82129 | — |
| 反応物 | 3-[(Tert-butyldimethylsilyl)oxy]propan-1-ol | HCID 4077791 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(t-Butyldimethylsilyloxy)-3-(p-nitrophenoxycarbonyloxy)propane | HCID 18939665 | — |
反応手順
A 0.604 g (3.00 mmol) sample of p-nitrophenoxycarbonylchloride in 3 mL of methylene chloride was added to a solution of 0.570 g (3.00 mmol) of 3-(t-butyldimethylsilyloxy)-l-propanol and 0.329 mL of 4-methylmorpholine in 2 mL of methylene chloride cooled in an ice bath. The solution was stirred for 2 hours. The mixture was diluted with methylene chloride, which was washed with water, dried and concentrated. The crude product was chromatographed on silica gel, eluting with 10% ethyl acetate in hexane. The solvent was removed and the product dried to afford 0.831 g of the title compound, which was taken directly to the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05837873 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-8da3edf749144590a330f676598eba7b |
| 出典メモ | uspto-grants-1998_11 |