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CAS No. : | 5325-64-4 | MDL No. : | MFCD00058283 |
Formula : | C3H9ClN2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | VVIXOTCTYAILNP-UHFFFAOYSA-N |
M.W : | 124.57 | Pubchem ID : | 13892956 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | To a solution of 3- [5-BROMO-4- [ (2, 4-difluorobenzyl) oxy]- 2-methyl-6-oxopyrimidin-1 (6H)-YL]-4-METHYLBENZOIC acid (1.0 g, 0.022 mol) in dimethylacetamide (10.0 mL) at-20 oC was added isobutylchloroformate (0.36 g, 0.0028 mol), followed by dropwise addition of N-METHYLMORPHOLINE (0.30 G, 0.003 mol) and stirred for 10 min under nitrogen atmosphere. The reaction mixture was then stirred at room temperature for 20 min, cooled to 0 oC, and added N-methylmorpholine (0.30 g, 0.003 mol) followed by the addition of N-methylglycine amide hydrochloride (0.35 G, 0.0028 mol) and DMAP (0.025 g). The reaction mixture was stirred at room temperature for 4 h, and concentrated IN VACUO. The resulting the residue was purified by reverse-phase HPLC using 10-90% CH3CN/Water gradient (40 min) at a flow rate of 80 mL/min. The appropriate fractions (MH+, m/z = 535) were combined, and freeze-dried to give a white solid. This was dissolved in dichloromethane (25 mL), washed successively with 5% sodium bicarbonate (2 x 20 mL), water (2 x 20 mL), dried (NA2SO4), and concentrated to dryness to afford the racemic title compound (0.75 g, 65%) as a white amorphous substance : 1H NMR (CD30D/400 MHz) 5 7.96 (dd 1H, J = 1.6 Hz, 8.0 Hz), 7.72 (d, 1H, J = 1.6 Hz), 7.62 (m, 1H), 7.56 (d, 1H, J = 8.0 Hz), 7.01 (m, 2H), 5.55 (abq, 2H), 3.99 (s, 2H), 2.74 (s, 3H), 2.18 (s, 3H), and 2.14 (s, 3H); ES-HRMS M/Z 535.0792 (M+H calcd for C23H22N404F2 Br requires 535. 0787). 19F NMR (CD3OD/ 400 MHz) -111. 85 (m) and - 115. 91 (m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
8.5 g (52%) | With sodium hydrogencarbonate; In water; benzene; | A solution of chloroacetyl chloride (0.1 mole, 11.3 g) in benzene (40 ml) was added over 30 min to a mixture of <strong>[5325-64-4]sarcosinamide hydrochloride</strong> (0.1 mole, 12.45 g) and sodium bicarbonate (0.25 mole, 20.0 g) in 40 ml of water. The mixture was vigorously stirred for 3 h at room temperature. The aqueous phase was acidified with 5M hydrochloric acid to pH 5 and extracted with ethyl acetate (3*400 ml). The combined extracts were dried over anhydrous sodium sulphate and evaporated in vacuo. The solid residue obtained was recrystallized from ethanol-ether to give 8.5 g (52%) of the title compound. Mp 85-86 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With methylamine; | EXAMPLE 87 PREPARATION OF alpha-CHLOROACETYLSARCOSINAMIDE Sarcosinamide hydrochloride was prepared by reacting methylamine with 2-chloroacetamide as described by Marvel et al. (1946). The compound was recrystallized from ethanol. Mp 160-161 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | To a solution of carbamoylmethyl-methyl-carbamic acid t-butyl ester (848 mg, 4.50 mmol) (obtained as described in Reference Example 44(1)) in 1,4-dioxane (8.50 ml) was added a solution of 4N hydrogen chloride in 1,4-dioxane (8.50 ml) in an ice bath, and the mixture was stirred at room temperature for 2.5 hours. After checking the completion of the reaction, diethyl ether was added thereto, and the reaction mixture was stirred for 30 minutes. The resulting reaction mixture was filtered, and the obtained residue was washed with diethyl ether and dried to give 2-methylaminoacetamide hydrochloride (421 mg, yield 75%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N-ethyl-N,N-diisopropylamine; sodium iodide; In N,N-dimethyl-formamide; at 160℃; for 0.0833333h;Microwave irradiation; | Example 16A 7-Chloro-1-(tetrahvdropyran-4-yl)methyl-3-(4-[Lambda/-(carboxamido)methyl-Lambda/- methylaminolmethylHI ,3l-thiazol-2-yl)-1 /-/-indole A mixture of 7-chloro-3-[4-(chloromethyl)thiazol-2-yl]-1-(tetrahydropyran-4- yl)methyl-1 /-/-indole (prepared as described in Example 16, using toluene-4-sulfonic acid tetrahydropyran-4-ylmethyl ester instead of cyclohexylmethyl bromide) (40 mg, 0.10 mmol), Lambda/-methyl glycine amide hydrochloride (18.4 mg, 0.15 mmol), di- isopropylethylamine (35 mul, 0.21 mmol) and sodium iodide (16 mg, 0.10 mmol) in dimethylformamide (2 ml) was subjected to microwave irradiation for 5 min at 160 C. The reaction mixture was filtered through a 5 g Strata SCX giga tube. The tube was washed with dichloromethane and then eluted with 10% (2 M ammonia in methanol) in dichloromethane. The product was purified by column chromatography eluting with 3:97 (v/v) (2M ammonia in methanol): dichloromethane to give the title compound (39 mg, 0.09 mmol). EsIMS: m/z 433.5, 435.4 [M+H]+. | |
With N-ethyl-N,N-diisopropylamine; sodium iodide; In N,N-dimethyl-formamide; at 160℃; for 0.0833333h;Microwave irradiation; | EXAMPLE 16A 7-Chloro-1-(tetrahydropyran-4-yl)methyl-3-(4-[N-(carboxamido)methyl-N-methylamino]methyl}-[1,3]-thiazol-2-yl)-1H-indole A mixture of 7-chloro-3-[4-(chloromethyl)thiazol-2-yl]-1-(tetrahydropyran-4-yl)methyl-1H-indole (prepared as described in Example 16, using toluene4-sulfonic acid tetrahydropyran4-ylmethyl ester instead of cyclohexylmethyl bromide) (40 mg, 0.10 mmol), N-methyl glycine amide hydrochloride (18.4 mg, 0.15 mmol), di-isopropylethylamine (35 mul, 0.21 mmol) and sodium iodide (16 mg, 0.10 mmol) in dimethylformamide (2 ml) was subjected to microwave irradiation for 5 min at 160 C. The reaction mixture was filtered through a 5 g Strata SCX giga tube. The tube was washed with dichloromethane and then eluted with 10% (2 M ammonia in methanol) in dichloromethane. The product was purified by column chromatography eluding with 3:97 (v/v) (2M ammonia in methanol): dichloromethane to give the title compound (39 mg, 0.09 mmol). EsIMS: m/z 433.5, 435.4 [M+H]+. |
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