Hydrochloric Acid → HCID 21285473, compound

A mixture comprising 2.86 g of the thiophenolate thus obtained, 30 ml of dried methanol and 3.0 ml of a 28% sodium methoxide methanol solution, was stirred at room temperature for 15 hours. Then, 1.5 ml of a 28% sodium methoxide methanol solution was added, and the mixture was stirred for further 5 hours. The reaction mixture was acidified to a pH of about 2 by gradually adding concentrated hydrochloric acid thereto, and then the solvent was distilled off. Water was poured into the dark brown oily residue thus obtained, and the mixture was extracted with benzene. The benzene layer was washed sequentially with water and a saturated sodium chloride aqueous solution, and dried over sodium sulfate. Then, the solvent was distilled off to obtain a dark brown oily substance. The oily substance was purified by silica gel column chromatograph by using benzene-n-hexane (2:1, v/v) as the developer, whereby 1.13 g of the above identified compound was obtained as a colorless oily substance.

1. customthus obtained
2. distillationthe solvent was distilled off
3. additionWater was poured into the dark brown oily residue
4. customthus obtained
5. extractionthe mixture was extracted with benzene
6. washThe benzene layer was washed sequentially with water
7. dry with materiala saturated sodium chloride aqueous solution, and dried over sodium sulfate
8. distillationThen, the solvent was distilled off
9. customto obtain a dark brown oily substance
10. customThe oily substance was purified by silica gel column chromatograph
11. customwas obtained as a colorless oily substance

ORD record

ord-083b80dd1ce948a9893bf496b701a137

Source dataset

uspto-grants-1988_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04783462