関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-Methyltetrahydrofuran | HCID 7301 | — |
| 反応物 | 4-Nitrophenyl chloroformate | HCID 82129 | — |
| 反応物 | 1-Phenylethanol, (R)- | HCID 637516 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Carbonic acid 4-nitro-phenyl ester (R)-1-phenyl-ethyl ester | HCID 11108942 | 98.3% |
反応手順
A mixture of (R)-1-phenyl-ethanol (60.6 g, 0.496 mol), pyridine (42.5 mL, 0.526 mol) and 2-methyl-tetrahydrofuran (600 mL) was cooled to 0° C. and p-nitrophenyl chloroformate (100 g, 0.496 mol) was added over 15 min keeping the internal temperature below 5° C. The reaction mixture was warmed to room temperature and stirred for 2 h. To the reaction mixture was added 1.0 M HCl in water (300 mL). Layers were separated. The organic layer was washed with 1N HCl (300 mL) and brine (300 mL), filtered, concentrated to dryness by rotary evaporation, and dried under vacuum to give the title compound (140 g) as a clear yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08101791B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-e9d41a3fd0764904b280ca3a75b9a963 |
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| 出典メモ | uspto-grants-2012_01 |
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