Hydrochloric Acid → 5-Chloromethylfurfural

To a three-necked flask equipped with a condenser and a stirrer were added 5 g (0.028 mole) of a commercially available D-glucose and two kinds of surface active agent, i.e., 97.6 mg (0.00028 mole) of sodium laurylbenzenesulfonate and 89.6 mg (0.00028 mole) of cetyltrimethylammonium chloride. Then, 30 ml of toluene was added thereto and the mixture was stirred to make a suspension. Thereafter, about 6 ml of 35% hydrochloric acid was slowly dropwise added from a dropping funnel over 1 hour with stirring. A slight excess of hydrogen chloride was then slowly passed therethrough at 45° C. over 3 hours with stirring. After stirring was continued for a further 4 hours, the reaction solution was diluted with a little water and filtered through Celite while being washed with toluene. The toluene layer was neutralized, dried and concentrated to obtain about 1.9 g of 5-chloromethylfurfural.

1. customTo a three-necked flask equipped with a condenser and a stirrer
2. stirringwith stirring
3. stirringat 45° C. over 3 hours with stirring
4. stirringAfter stirring
5. filtrationfiltered through Celite
6. washwhile being washed with toluene
7. customdried
8. concentrationconcentrated

ORDレコード

ord-06ec1e8c1cd547ffad15da46e304360d

出典データセット

uspto-grants-1979_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04154744