Related Products of 875251-47-1 , The common heterocyclic compound, 875251-47-1, name is 2-(Pyrimidin-5-yl)ethanol, molecular formula is C6H8N2O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
[0715] Synthesis of 5-(2-chloroethyl) pyrimidine: [0716] To a stirred solution of 2-(pyrimidin-5-yl) ethanol (20 mg, 0.16 mmol) in CH2CI2 (4 mL) under argon atmosphere was added sulfurous dichloride (0.02 mL, 0.32 mmol) at 0 C; heated to 50 C and stirred for 4 h. The reaction was monitored by TLC; after completion of the reaction, the reaction mass was cooled to room temperature and pH was adjusted to ~8 using saturated NaHC03 solution( 5 mL) and the compound was extracted with CH2CI2 (2 x 10 mL). The combined organic extracts were dried over sodium sulphate, filtered and concentrated in vacuo to obtain the crude. The crude was purified through silica gel column chromatography using 2% MeOH/ CH2C12 to afford 5-(2-chloroethyl) pyrimidine (18 mg, 77%) as colorless syrup. [0717] 1H-NMR (CDC13, 400 MHz): delta 9.16 (s, 1H), 8.66 (s, 2H), 3.78 (t, 2H), 3.12 (t, 2H); LC-MS: 97.54%; 143 (M++l); (column; Xbridge C-18, 50 3.0 mm, 3.5 mupiiota); RT 1.80 min. 0.05% TFA (aq.): ACN; 0.8 mL/min); UPLC (purity): 99.22%; (column: Acquity BEH C-18, 50 x 2.1 mm, 1.7 mu); RT 1.15 min. ACN : 0.025% TFA (Aq); 0.5 mL/min. (IP12060335); TLC: 10% MeOH/ CH2C12 (Rf: 0.7).
The synthetic route of 875251-47-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ENVIVO PHARMACEUTICALS, INC.; RIPKA, Amy; SHAPIRO, Gideon; MCRINER, Andrew, J.; BURSAVICH, Matthew, Gregory; WO2013/142269; (2013); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia