Diethylamine → HCID 85604371、化合物

To a solution of 5-methylhex-2-enoic acid (formula-3) (20 grams) in dichloromethane (250 ml), 2 ml of dimethyl formamide was added. To this mixture thionyl chloride (24.1 grams) was added. The reaction mixture was stirred for 2.5 hours at 28-29° C. The reaction mixture was cooled to 0-5° C. and diethyl amine was added to the reaction mixture at 5-8° C. until the pH reached to 8.5. The reaction mixture was stirred for 1.5 hours at 0-5° C. The reaction mixture was quenched with water. Separated the aqueous and organic layers. The organic layer was washed with 5% sodium bicarbonate solution and was dried over anhydrous sodium sulphate. The solvent was distilled off completely under vacuum to provide the title compound as solid.

1. temperatureThe reaction mixture was cooled to 0-5° C.
2. stirringThe reaction mixture was stirred for 1.5 hours at 0-5° C
3. customThe reaction mixture was quenched with water
4. customSeparated the aqueous and organic layers
5. washThe organic layer was washed with 5% sodium bicarbonate solution
6. dry with materialwas dried over anhydrous sodium sulphate
7. distillationThe solvent was distilled off completely under vacuum

ORDレコード

ord-86e8700bcc074694aaa7c48f97eeb7be

出典データセット

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08168828B2