HCID 19989233, compound → HCID 19989223, compound

To a suspension of the product obtained in Step 2 (3.5 g) was dropwise added 8.6 ml of 1M sodium ethoxide ethanol solution with vigorous stirring under ice cooling over a period of ten minutes. The mixture was stirred at room temperature for one hour, and the resulting yellow solution was concentrated under reduced pressure. The remaining yellow oil was shaken with 100 ml of chloroform and 50 ml of water. The chloroform layer was separated and the aqueous layer was again extracted with 100 ml of fresh chloroform. The chloroform layers were joined and washed with 100 ml of saturated sodium chloride solution and dried over anhydrous sodium sulfate. The chloroform solution was concentrated under reduced pressure, and 20 ml of n-hexane was added to the concentrate to give 1.8 g of the objective compound as faint yellow crystals.

1. stirringThe mixture was stirred at room temperature for one hour
2. concentrationthe resulting yellow solution was concentrated under reduced pressure
3. stirringThe remaining yellow oil was shaken with 100 ml of chloroform and 50 ml of water
4. customThe chloroform layer was separated
5. extractionthe aqueous layer was again extracted with 100 ml of fresh chloroform
6. washwashed with 100 ml of saturated sodium chloride solution
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationThe chloroform solution was concentrated under reduced pressure, and 20 ml of n-hexane
9. additionwas added to the
10. concentrationconcentrate

ORD record

ord-ee5883c330564da6abd2f9167a0f0950

Source dataset

uspto-grants-1989_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04888332