Statistics shows that 71670-70-7 is playing an increasingly important role. we look forward to future research findings about 2-(Chloromethyl)-5-methylpyridine hydrochloride.
Reference of 71670-70-7, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.71670-70-7, name is 2-(Chloromethyl)-5-methylpyridine hydrochloride, molecular formula is C7H9Cl2N, molecular weight is 178.06, as common compound, the synthetic route is as follows.
Step 3: 4-{[(5-Methylpyridin-2-yl)methyl]oxy}aniline dihydrochloride N-(4-Hydroxyphenyl)acetamide (25.0 kg) and potassium carbonate (50.0 kg) were mixed in ethanol (187.5 L) at 22±3 C. and 2-(chloromethyl)-5-methylpyridine hydrochloride (32.5 kg) was added portionwise at 22±3 C. The mixture was then heated to reflux for 15 h. The reaction was then cooled to 57±3 C. and water (162.5 L) added maintaining this temperature. The organic and aqueous phases were allowed to separate and the lower aqueous layer was removed. The organic layer was then washed with aqueous potassium carbonate (20% w/v, 114 kg) at 57±3 C. Sodium hydroxide (50% w/v, 57.8 kg) was then added together with ethanol (12.5 L) and the reaction stirred at reflux for about 38 h. The reaction was cooled to 57±3 C. and the lower aqueous phase was removed. The organic layer was concentrated to ~125 L by atmospheric distillation, 2-butanol (250 L) was then added and the concentration repeated. The reaction was then cooled to 22±3 C., further 2-butanol (125 L) was added and the mixture washed with water (75 L) at 50±3 C., followed by aqueous sodium chloride (5% w/w, 78 kg) at 50±3 C. The reaction was concentrated to 125 L by atmospheric distillation, further 2-butanol (125 L) was then added and the concentration repeated. 2-Propanol (150 L) was then added followed by hydrogen chloride (5 M -6 M in 2-propanol, 89.5 kg) over 2 hours at 76±3 C. The resulting slurry was then cooled to 22±3 C. over about 3.5 h, aged for about 40 min and the product isolated by filtration, washed with 2-propanol (2*200 L) follow by TBME (200 L) and dried at 40-50 C. under vacuum to give the title product (40.25 kg, 85% th). 1H NMR (400 MHz, DMSO-D6) deltappm 8.74 (1H, s); 8.28 (1H, dd, J=8.2, 1.3 Hz); 7.91 (1H, d, J=8.1 Hz); 7.38-7.42 (2H, m); 7.17-7.21 (2H, m); 5.46 (2H, s); 2.45 (3H, s).
Statistics shows that 71670-70-7 is playing an increasingly important role. we look forward to future research findings about 2-(Chloromethyl)-5-methylpyridine hydrochloride.
Reference:
Patent; Crawford, Claire Frances; Garcia, Sandrine; Graham, Jonathan Paul; Harling, Sandra Jane; Henley, Nicholas Paul; Hermitage, Stephen Andrew; Hutchinson, John Howard; Keel, Trevor Raymond; Kennedy, Andrew; Mason, Andrew McMurtrie; Scott, Mark Simon; Smith, Neil Michael; Stock, Nicholas Simon; Tateno, Yuichi; Trouw, Leontine Saskia; Turner, Peter Graham; Wallis, Christopher John; Willacy, Robert David; US2012/220779; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem