Methanol → HCID 18358023, compound

The reaction was effected as described in Example 49, but using 92 mg of methyl N-[5-(1,2-dithiolan-3-yl)pentyl]oxcalamidate (prepared as described in Example 65), 4 ml of methanol, 1 ml of tetrahydrofuran and 0.6 ml of a 1N aqueous solution of sodium hydroxide. The solvent was removed from the reaction mixture by distillation under reduced pressure. Water was added to the residue. The resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid, after which it was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate. Ethyl acetate was removed from the extract by distillation under reduced pressure. The residue was dissolved in dioxane, after which it was lyophilised, to give 64 mg of the title compound as a pale yellow amorphous substrate, melting at 75 to 79° C.

1. customThe solvent was removed from the reaction mixture by distillation under reduced pressure
2. additionWater was added to the residue
3. additionThe resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid
4. extractionafter which it was extracted with ethyl acetate
5. washThe extract was washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous sodium sulfate
7. customEthyl acetate was removed from the
8. extractionextract by distillation under reduced pressure
9. dissolutionThe residue was dissolved in dioxane

ORD record

ord-44411f13e8a347a4b0de109f5bd2d371

Source dataset

uspto-grants-2000_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06013663