Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 2854-16-2, name is 1-Amino-2-methylpropan-2-ol. A new synthetic method of this compound is introduced below., Quality Control of 1-Amino-2-methylpropan-2-ol
Example 82N-(2-{[(2-hydroxy-2-methylpropyl)amino]methyl}-1,7-dimethyl-1H-indol-6-yl)-4-[(2S)-tetrahydrofuran-2-ylmethoxy]benzamideN-(2-Formyl-1,7-dimethyl-1H-indol-6-yl)-4-[(2S)-tetrahydrofuran-2-ylmethoxy]benzamide (300 mg) obtained in Reference Example 66, 1-amino-2-methylpropan-2-ol (102 mg) and acetic acid (1.53 mL) were added to N,N-dimethylacetamide (5 mL), and the mixture was stirred at room temperature for 1 hr.Sodium triacetoxyborohydride (324 mg) was added, and the mixture was stirred at room temperature for 21 hr. 8N Aqueous sodium hydroxide solution (3.82 mL) was added dropwise at 0°C.The mixture was extracted with ethyl acetate, washed with brine, dried over anhydrous sodium sulfate, purified by silica gel column chromatography [eluent; ethyl acetate_methanol=100:0 (volume ratio)?methyl acetate_methanol=60:40 (volume ratio)], and crystallized from ethyl acetate and diisopropyl ether to give the title compound (289 mg, yield 81percent) as a beige solid.1H NHR (300 MHz, DMSO-d6) delta: 1.10 (6 H, s), 1.59 – 2.10 (4 H, m), 2.46 (2 H, s), 2.55 (3 H, s), 3.65 – 3.74 (1 H, m), 3.76 – 3.85 (1 H, m), 3.87 (2 H, s), 3.96 – 4.12 (5 H, m), 4.13 – 4.25 (2 H, m), 6.29 (1 H, s), 6.82 (1 H, d, J=8.3 Hz), 7.05 (2 H, d, J=8.7 Hz), 7.26 (1 H, d, J=8.3 Hz), 7.98 (2 H, d, J=8.7 Hz), 9.80 (1 H, s).melting point: 197-200°Celemental analysis (C27H35N3O4*0.2H2O)Calculated: C, 69.12; H, 7.60; N, 8.96.Found: C, 69.06; H, 7.41; N, 8.83.
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Reference:
Patent; Takeda Pharmaceutical Company Limited; EP2522657; (2012); A1;,
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