Butanoyl chloride, 2-methyl- → Tert-butyl 2-methylbutanoate

温度

0 °C

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).

1. additionAfter the addition
2. customat RT for h, and about half of the solvent was then removed under reduced pressure
3. additionAfter addition of diethyl ether, sat. sodium bicarbonate solution
4. additionwas added dropwise with vigorous stirring
5. customAfter phase separation
6. extractionthe aqueous phase was extracted with diethyl ether
7. washthe combined organic phases were washed with sat. sodium carbonate solution
8. dry with materialdried over sodium sulphate
9. concentrationconcentrated under reduced pressure
10. distillationThe crude product was purified by vacuum distillation (19 mm Hg, 40-45° C.)

ORDレコード

ord-c2b13b313e564c8fb82b927cd1a695ee

出典データセット

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09018414B2