Water → HCID 57827343、化合物

4,4-Dimethoxybutyraldehyde (Org. Biomol. Chem. 4 (2006) 2158) (5.47 g) was dissolved in THF (55 mL), and the solution was cooled in an ice bath under a nitrogen atmosphere. Then, a solution of allylmagnesium chloride in THF (62.1 mL, 1 M) was slowly added. After completion of the addition, the mixture was stirred for three hours. After slowly adding water, ethyl acetate and a saturated ammonium chloride solution were added, followed by further stirring. The aqueous layer was separated and then the organic layer was sequentially washed with a saturated ammonium chloride solution, water and brine. The resulting organic layer was dried over anhydrous magnesium sulfate, and the solid was removed by filtration. The filtrate was concentrated under reduced pressure and then purified by silica gel column chromatography to obtain the title compound (5.55 g).

1. temperaturethe solution was cooled in an ice bath under a nitrogen atmosphere
2. additionAfter completion of the addition
3. customThe aqueous layer was separated
4. washthe organic layer was sequentially washed with a saturated ammonium chloride solution, water and brine
5. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
6. customthe solid was removed by filtration
7. concentrationThe filtrate was concentrated under reduced pressure
8. custompurified by silica gel column chromatography

ORDレコード

ord-693cc51543354507b705d27bf9be960f

出典データセット

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08946211B2