関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 3-[(Tert-butyldimethylsilyl)oxy]propan-1-ol | HCID 4077791 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-((Tert-butyldimethylsilyl)oxy)propanal | HCID 3662392 | — |
反応手順
DMSO (24 mmol) is added to oxalyl chloride (11 mmol) in 40 mL of CH2Cl2 cooled to −78° C. After 15 minutes, alcohol 46 (10 mmol) is added. After an additional 15 minutes, triethylamine (50 mmol) is added. The mixture is allowed to warm to 0° C. and then poured into 0.1 M HCl (100 mL). The phases are separated, and the aqueous phase is extracted with ethyl acetate (2×100 mL). The organic phases are washed with water (100 mL), dried over anhydrous MgSO4, and concentrated in vacuo. The mixture is purified by flash chromatography to give the product as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06702705B1 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-5c15f2fb99da45d49beebf1bfbf5498f |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|
