1,2-Ethanedithiol → 1-Propanol, 3,3'-[1,2-ethanediylbis(thio)]bis-

To 300 ml of absolute methanol, was added 12.2 g of metallic sodium. To the resulting solution which was being stirred in an ice bath, was added dropwise 25 g of dithioglycol. After the dropwise addition, the stirring was continued for additional 30 minutes in the ice bath. Then, 52 g of 3-chloro-1-propanol was further added dropwise. At the conclusion of the dropwise addition, the temperature of the reaction system was raised to a room temperature, and the reaction system was allowed to stand for 10 hours at the room temperature. The thus produced sodium chloride was removed by filtration under reduced pressure, and the resulting filtrate was concentrated. Crystals thus obtained were recrystallized from acetone. Melting Point 52° C., Yield 20 g.

1. additionAfter the dropwise addition
2. additionAt the conclusion of the dropwise addition
3. customThe thus produced sodium chloride was removed by filtration under reduced pressure
4. concentrationthe resulting filtrate was concentrated
5. customCrystals thus obtained
6. customwere recrystallized from acetone

ORD record

ord-58774d7ce4e248c197c047be0bbd9f3e

Source dataset

uspto-grants-1985_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04551419