Chloroform → HCID 19063201, compound

1.07 g (5.0 mmol) of compound 001C, which had been prepared in Step C of Reference Example 1, was dissolved in 11 ml of acetonitrile. To the resultant solution were added 1.64 ml (15.0 mmol) of benzylamine and 2.07 g (15.0 mmol) of potassium carbonate. The resultant mixture was stirred at 80° C. for 8 hours to effect a reaction. To the resultant reaction mixture was added 100 ml of chloroform to obtain a mixture. The obtained mixture was successively washed with 100 ml of water and 100 ml of saturated saline, to thereby form a chloroform layer containing the desired compound 002A, followed by separation of the chloroform layer. The chloroform layer thus separated was dehydrated by means of a Whatman 1PS filter paper and then, concentrated in vacuo to thereby obtain a residue. The obtained residue was purified by silica gel column chromatography. That is, the residue was applied to a column of 50 g of silica gel (Art. 9385, manufactured and sold by E. Merck, Darmstadt, Germany) and eluted with chloroform, to thereby obtain 873 mg of compound 002A as a yellow oily substance (yield: 73%).

1. customa reaction
2. customTo the resultant reaction mixture
3. customto obtain a mixture
4. washThe obtained mixture was successively washed with 100 ml of water and 100 ml of saturated saline
5. customto thereby form a chloroform layer
6. customfollowed by separation of the chloroform layer
7. customThe chloroform layer thus separated
8. filtrationfilter paper
9. concentrationconcentrated in vacuo
10. customto thereby obtain a residue
11. customThe obtained residue was purified by silica gel column chromatography
12. washeluted with chloroform

ORD record

ord-8e676fd53e374d0f9e0412f4a0c73b1a

Source dataset

uspto-grants-1998_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05798382