Dimethylamine → HCID 76281363, Verbindung

To a stirred solution of 74 (2 g, 5.7 mmol) in acetonitrile (10 mL) was added sodium bicarbonate (0.48 g, 5.74 mmol) and followed by dimethyl amine (40% in water) (10 mL, 88.8 mmol) at 25-30° C. The reaction mixture was stirred for 3 hours at 25-30° C.; the reaction was monitored by TLC. The solid obtained in the reaction mixture was filtered under vacuum. The solvent was concentrated, diluted with ethyl acetate/water and stirred for 15 minutes at 25-30° C. The aqueous and organic layers were separated, and the aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic layers were washed with brine solution. The organic layer was dried over Na2SO4 and concentrated under vacuum to afford crude 75 (1.49 g, yield: 83%) as a liquid.

1. customThe solid obtained in the reaction mixture
2. filtrationwas filtered under vacuum
3. concentrationThe solvent was concentrated
4. additiondiluted with ethyl acetate/water
5. stirringstirred for 15 minutes at 25-30° C
6. customThe aqueous and organic layers were separated
7. extractionthe aqueous layer was extracted with ethyl acetate (2×10 mL)
8. washThe combined organic layers were washed with brine solution
9. dry with materialThe organic layer was dried over Na2SO4
10. concentrationconcentrated under vacuum

ORD-Eintrag

ord-bbb9a45045894ec589f0483fe67f7b73

Quelldatensatz

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08900625B2