Sodium Hydroxide → HCID 18765916, compound

The solution of ethyl 3-(2-{[2-(1-pyrrolidinyl)ethoxy]methyl}phenyl)propanoate (8.10 g, 26.5 mmol) in ethanol (40 ml) and 5N NaOH aq. solution (32.0 mmol, 6.4 ml) was stirred at room temperature for 15 h. The mixture was neutrallized with 1N HCl-ethanol (32 ml) at 0° C. The solvents were removed by simple distillation procedure at ˜1 atom (oil bath temperature; 105˜110° C.). The residue was then diluted with acetonitrile (50 ml) and then the solvents were removed by distillation (oil bath temperature; 105˜110° C.) for azeotropic removal of water and ethanol until inner temperature 79.5° C.˜80.5° C. The residue was then diluted with acetonitrile (60 ml) and dried over sodium sulfate. After filtration, the filtrate was evaporated in vacuo to afford the titled compound (quant.) as a dark yellow oil.

1. customThe solvents were removed by simple distillation procedure at ˜1 atom (oil bath temperature; 105˜110° C.)
2. additionThe residue was then diluted with acetonitrile (50 ml)
3. customthe solvents were removed by distillation (oil bath temperature; 105˜110° C.) for azeotropic removal of water and ethanol until inner temperature 79.5° C.˜80.5° C
4. additionThe residue was then diluted with acetonitrile (60 ml)
5. dry with materialdried over sodium sulfate
6. filtrationAfter filtration
7. customthe filtrate was evaporated in vacuo

ORD record

ord-cb523ae6295f4999976efef26a98477f

Source dataset

uspto-grants-2003_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06653313B2