(2,2-Dimethyl-1,3-dithiolan-4-yl)methanol → 1,3-Dithiolane, 4-(chloromethyl)-2,2-dimethyl-

To a solution of 3.46 g (0.021 mole) of 2,2-dimethyl-4-hydroxymethyl-1,3-dithiolan in 15 mL of toluene was added dropwise 2.35 g (0.020 mole) of thionyl chloride, and the mixture was heated gradually to 80°-85° C., maintained at that temperature for 0.75 hour, then stirred at room temperature for 16 hours. The mixture was filtered, and the filtrate concentrated to dryness at 60° C./100 mm Hg to give a residual oil. Distillation of the oil gave 1.81 g of product, bp 75°-78° C./1.25-1.35 mm Hg.

1. temperaturethe mixture was heated gradually to 80°-85° C.
2. temperaturemaintained at that temperature for 0.75 hour
3. filtrationThe mixture was filtered
4. concentrationthe filtrate concentrated to dryness at 60° C./100 mm Hg
5. customto give a residual oil
6. distillationDistillation of the oil

ORDレコード

ord-0669c09553f140b38c9ed133c4840ed6

出典データセット

uspto-grants-1987_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04702763