Hydrochloric Acid → 5-Hydroxy-1,3-dimethyl-tetrahydro-pyrimidin-2-one

Temperature

70 °C

To a solution of 1,3-dimethyl-5-triisopropylsilanyloxy-tetrahydro-pyrimidin-2-one (Step P8) (9.1 g, 28 mmol) in EtOH (70 mL) was added a 1M HCl (140 mL, 140 mmol) and the mixture was stirred for 3 h at 70° C. The mixture was concentrated, and the pH of the resulting aqueous phase was adjusted to 5 with a saturated aqueous NaHCO3 solution. The aqueous layer was saturated with NaCl and was extracted with CH2Cl2/isopropanol 3:1. The organic layer was dried (Na2SO4), filtered and concentrated to afford the title compound. ESI-MS: tR=0.33 min, [M+H]+ 145.1 (LC-MS 1).

1. concentrationThe mixture was concentrated
2. extractionwas extracted with CH2Cl2/isopropanol 3:1
3. dry with materialThe organic layer was dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated

ORD record

ord-23ad60b1c589492e9eef7f5f279e4ade

Source dataset

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09365576B2