Triphenylphosphine → HCID 86760470, Verbindung

Temperatur

0 °C

To a 250-mL dry, round-bottomed flask was added 3-(2,6-Difluoro-3,5-dimethoxy-phenyl)-7-methylsulfanyl-2-oxo-3,4-dihydro-2H-pyrimido[4,5-d]pyrimidine (1.5 g, 4.08 mmol), ethyl-4-hydroxycyclohexanecarboxylate (2.11 g, 12.23 mmol), triphenylphosphine (3.21 g, 12.23 mmol), and tetrahydrofuran (50 mL), and the solution was blanketed with a nitrogen atmosphere. The solution was then cooled to 0° C., and diisopropylazodicarboxylate (2.41 mL, 12.23 mmol) was added dropwise. The solution was then warmed to room temperature and stirred overnight. The crude mixture was then concentrated in vacuo and taken up in dichloromethane, washed with water, dried over sodium sulfate, and concentrated. The crude was purified by flash silica chromatography eluting with 3:2 hexane/ethyl acetate to yield the title compound (1.17 g, 55% yield): LRMS: 523.2 (M+H).

1. customTo a 250-mL dry
2. temperatureThe solution was then warmed to room temperature
3. concentrationThe crude mixture was then concentrated in vacuo
4. washwashed with water
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe crude was purified by flash silica chromatography
8. washeluting with 3:2 hexane/ethyl acetate

ORD-Eintrag

ord-9e54ba409d1a4d71ac46dcacd7d47e46

Quelldatensatz

uspto-grants-2007_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07196090B2