関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butanoyl chloride, 2-methyl- | HCID 93697 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Tert-butyl 2-methylbutanoate | HCID 523483 | 32.3% |
反応手順
15.0 g (124.4 mmol) of 2-methylbutyryl chloride were dissolved in 150 ml of abs. THF and cooled to 0° C., and 114 ml (114 mmol) of a 1 M solution of potassium tert-butylate in THF were added dropwise. After the addition had ended, the mixture was stirred at 0° C. for 1 h and then at RT for h, and about half of the solvent was then removed under reduced pressure. After addition of diethyl ether, sat. sodium bicarbonate solution was added dropwise with vigorous stirring. After phase separation, the aqueous phase was extracted with diethyl ether, and the combined organic phases were washed with sat. sodium carbonate solution, dried over sodium sulphate and concentrated under reduced pressure. The crude product was purified by vacuum distillation (19 mm Hg, 40-45° C.). This gave a total of 6.35 g of the target product (32.3% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09018414B2 |
|---|
| 出典データセット | uspto-grants-2015_04 |
|---|
| ORD ID | ord-c2b13b313e564c8fb82b927cd1a695ee |
|---|
| 出典メモ | uspto-grants-2015_04 |
|---|