Sodium Hydroxide → HCID 12954121, compound

0.74 ml (0.007 mol) of 1-chloroethyl chloroformate is added to a solution of 1.6 g (0.006 mol) of 8-(phenylmethyl)-1,4-dithia-8-azaspiro-[4.5]decane in 20 ml of dichloroethane; the mixture is heated under reflux for 1.5 h, it is cooled to room temperature, 8 ml of 1 M sodium hydroxide are added, the organic phase is decanted off, the aqueous phase is washed with 25 ml of dichloromethane, the organic phases are dried with sodium sulphate and then evaporated to dryness; the residue is dissolved in 35 ml of methanol and the solution is heated at 60° C. for 40 min; the solvent is evaporated off and the solid obtained is triturated with diisopropyl ether; 0.993 g of 1,4-dithia-8-azaspiro[4.5]decane hydrochloride is thus obtained in the form of a white solid. Yield 78%. Melting point >250° C.

1. temperaturethe mixture is heated
2. temperatureunder reflux for 1.5 h
3. customthe organic phase is decanted off
4. washthe aqueous phase is washed with 25 ml of dichloromethane
5. dry with materialthe organic phases are dried with sodium sulphate
6. customevaporated to dryness
7. dissolutionthe residue is dissolved in 35 ml of methanol
8. temperaturethe solution is heated at 60° C. for 40 min
9. customthe solvent is evaporated off
10. customthe solid obtained
11. customis triturated with diisopropyl ether

ORD record

ord-969f645931924c1f924ea9000bfc4da8

Source dataset

uspto-grants-2001_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06262060B1