関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 1,2-Pyrrolidinedicarboxylic acid, 1-(1,1-dimethylethyl) ester, (2S)- | HCID 85083 | — |
| 反応物 | 1,1,2-Trichloroethanol | HCID 119427 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 生成物 | HCID 10665296 | HCID 10665296 | — |
反応手順
Boc-Pro-OH (6.46 g, 30.0 mmol) in a 300 ml short neck flask was dissolved in distilled CHCl3 (80 ml). DCC (6.82 g, 33.0 mmol) dissolved in advance in a minimum quantity of distilled CHCl3 in ice bath with stirring was added thereto, and trichloroethanol (3.50 ml, 37.0 mmol) and DMAP (0.38 g, 3.0 mmol) was further added, and the mixture was stirred in an ice bath for 2 hours and at room temperature all day. After filter-out of DCUrea, the filtrate was subjected to vacuum concentration. The residue was dissolved in AcOEt, was sequentially washed with a 10% aqueous citric acid solution, water, a saturated aqueous NaHCO3 solution, water, and saturated saline, and was dried with Na2SO4. The filtrate was subjected to vacuum concentration to yield an oil-form product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07713926B2 |
|---|
| 出典データセット | uspto-grants-2010_05 |
|---|
| ORD ID | ord-47a9cb95990545e781cca9dd1e0690b5 |
|---|
| 出典メモ | uspto-grants-2010_05 |
|---|