Ethane, 1-chloro-2-ethoxy- → HCID 19806348, compound

Dissolved in 2.5 ml of N,N-dimethylformamide were 0.50 g of 2-mercapto-4-(3-pyridyl)-thiazole oxalate (1.82 mmol), and 0.10 g (4.17 mmol) of sodium hydride were added to the solution, which was stirred at room temperature. One hour later, 0.40 ml (3.65 mmol) of 2-chloroethyl ethyl ether were added to the suspension, which was then stirred for 2 hours at 80° C. The reaction solution was diluted with 50 ml of chloroform, followed by addition of 50 ml of a 5% saline solution and washing. After separation of the chloroform layer, the organic layer was dried over anhydrous magnesium sulfate, and concentrated in vacuo. The residues were then purified by silica gel chromatography to obtain 45 g of the title compound as an yellow oily form (93% yield).

1. additionwere added to the solution, which
2. stirringwas then stirred for 2 hours at 80° C
3. additionfollowed by addition of 50 ml of a 5% saline solution
4. washwashing
5. customAfter separation of the chloroform layer
6. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo
8. customThe residues were then purified by silica gel chromatography

ORD record

ord-927fbf6520ad4aeb880e79b30bb805ac

Source dataset

uspto-grants-1992_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05171746