Triethylamine → HCID 20800560, 화합물

2-(2-Hydroxy-1-phenyl-ethyl)-5-methyl-2,3-dihydro-isoindol-1-one (4.72 g, 17.66 mmol) and triethylamine (5.36 g, 53.97 mmol, 7.38 mL) were taken up in anhydrous DCM (50 mL), under argon and cooled to 0° C. Methanesulfonyl chloride (2.22 g, 19.43 mmol, 1.5 mL) was added to the reaction over 10 min. The reaction was stirred for 1 h at 0° C. then allowed to slowly warm to room temp and stirred for 4 h. The reaction was slowly poured into saturated sodium bicarbonate and the aqueous layer was extracted three times with ethyl acetate. The combined organic layers were washed with 1N HCl, water, brine and dried over anhydrous magnesium sulfate. The solution was filtered and the solvent removed under reduced pressure. The product was used in the next step without further purification. Yield 5.61 g.

1. temperatureto slowly warm to room temp
2. stirringstirred for 4 h
3. extractionthe aqueous layer was extracted three times with ethyl acetate
4. washThe combined organic layers were washed with 1N HCl, water, brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe solution was filtered
7. customthe solvent removed under reduced pressure
8. customThe product was used in the next step without further purification

ORD 기록

ord-ec3d3b3e1691428f84030a62b496d09e

출처 데이터셋

uspto-grants-2005_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06906067B2