Hydrochloric Acid → HCID 54433002, compound

Temperature

70 °C

Into a solution of 18.4g of thioglycolic acid in 50cc of water neutralized by 16g of NaOH in 60cc of water, there is poured a solution of 33.1g of 1,1-diethyl-3-hydroxy azetidinium chloride in 90cc of water. The resulting mixture is heated for 5 hours at 70° C under a nitrogen atmosphere, at which time it is then neutralized by the addition thereto of 16.5cc of 12N HCl. The water is then expelled by distilling the reaction mixture under a vacuum and the residue is then taken up in 200cc of isopropanol. After eliminating the sodium chloride precipitate by filtration, the resulting alcoholic filtrate is evaporated to dryness. The residue is then taken up in 100cc of water and filtered through a bed of DOWEX50W resin in order to eliminate residual traces of sodium chloride. The thus treated aqueous solution is then evaporated to dryness yielding an oil which when treated with acetone provides 29.2g of a whitish product melting at 104° C.

1. additionis then neutralized by the addition
2. distillationby distilling the reaction mixture under a vacuum
3. filtrationby filtration
4. customthe resulting alcoholic filtrate is evaporated to dryness
5. filtrationfiltered through a bed of DOWEX50W resin in order
6. customThe thus treated aqueous solution is then evaporated to dryness
7. customyielding an oil which when

ORD record

ord-85a3c31cb5ef4609a4d22328a9312de5

Source dataset

uspto-grants-1978_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04087550