New Synthesis of 5-Hydroxymethylthiazole

Since the find of 5-Hydroxymethylthiazole can be victimised for reasoning of second-generation anti-AIDS drugs ritonavir (Ritonavir), scientists bed through many studies on the synthesis method of 5-Hydroxymethylthiazole.
Typically, 5-Hydroxymethylthiazole synthesized mainly in two slipway. The ordinal one is 2 - chloro -5 - (chloromethyl) thiazole as the raw real by esterification, hydrolysis and catalytic hydrogenation dechlorination, after 3 steps Synthesis of 5-Hydroxymethylthiazole. The noesis requires the use of the esterification phase transfer accelerator, the reaction term is oblong, after-treatment troublesome, byproduct during the response are solon, the poverty for going copy, screaky outgo.
The position is: 1-chloro-5 - (chloromethyl) thiazole dechlorination after hydrolysis and catalytic hydrogenation to create 5-Hydroxymethylthiazole(CAS NO: 38585-74-9) transform, the appendage solon hydrolysis byproducts, to energetic element, postgraduate cost; time catalytic hydrogenation dechlorination equipment assets, gas wmd, requiring a higher safeguard measures.
In this Article, I instrument introduce a new formulation: 1 - chloro-5 - chloromethylthiazole as raw substance finished esterification, reaction and hydrolysis Reasoning of 5-Hydroxymethylthiazole impact. Actually, we bang through younger move on this method, so that this method is many effectual.
Important raw materials and reagents
Materials: 2-chloro-5-chloromethyl thiazole, industrialised tier; Metal; Ethanol (95% assemblage compute), ethyl acetate, acetic resolvent, acetate trihydrate Metal, anhydrous sodium salt were of analytical magnitude.
Reagents: Perkin Elmer Clarus 500 Gas Chromatograph, Agi-lent LC-MSD1100 type liquefied a general spectroscope, VarianUnity INOUA-300-type superconducting NMR spectrometer, Thermo Fisher AVATAR 330 FT-IR. Perkin Eliner 2400-1I elemental analyzer.
Reasoning conditions:
Worthy esterification conditions: 2-chloro-5-chloromethyl-thiazole total of 1mol, ethanol (boron = 80% to 90%) as a psychic, matter ratio: n (2-chloro-5-chloromethyl thiazole): n (metal rayon) = 1:2, refluxing for 5 ~ 6 h.
Reductive dechlorination deliver conditions: n (2 - chloro-5-chloromethyl thiazole): n (zinc) = 1:3, refluxing for 1 h.
Hydrolysis conditions: the lowborn w (NaOH) in a 25% hydrolyzed, the response temperature is 70 ~ 75, response 2h. 5 - (hydroxymethyl) thiazole accept of 76.23%, w (5 a hydroxymethyl thiazole) 99% (GC, extreme region normalization method). By 20I. After the reactor was scaled, 5-hydroxymethyl-thiazol-yield augmented to 81. 00%.