Sodium Hydroxide → HCID 20330460, compound

The thioureido compound (8 gm.) from Step B was refluxed in 50 ml. absolute ethanolic sodium hydroxide (6.5% w/v) for 4 hours under nitrogen, cooled and evaporated to dryness. The residue was dissolved in 50 ml. of water and 50 ml. of glacial acetic acid and evaporated to near dryness, and extracted with 4 × 40 ml. of chloroform. The chloroform was washed with 1 × 20 ml. of water, dried over magnesium sulfate, and treated with gaseous hydrogen chloride. The precipitate was collected, washed with acetone and dried to give 2.0 g. of 3-mercaptomethylpyridine-N-oxide hydrochloride, m.p. 184°-190°C.

1. temperaturecooled
2. customevaporated to dryness
3. dissolutionThe residue was dissolved in 50 ml
4. customof glacial acetic acid and evaporated
5. extractionextracted with 4 × 40 ml
6. washThe chloroform was washed with 1 × 20 ml
7. dry with materialof water, dried over magnesium sulfate
8. additiontreated with gaseous hydrogen chloride
9. customThe precipitate was collected
10. washwashed with acetone
11. customdried
12. customto give 2.0 g

ORD record

ord-4a1aeaa680ff4e41947ba749ee398876

Source dataset

uspto-grants-1976_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03971797