D-Proline, 1,2-dimethyl- synthesis
- Product Name:D-Proline, 1,2-dimethyl-
- CAS Number:1268520-34-8
- Molecular formula:C7H13NO2
- Molecular Weight:143.18
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Yield:1268520-34-8 100%
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen in methanol;water; under 1551.49 Torr; for 48 h;
Steps:
1 Step 1. Synthesis of 1,2-dimethyl-D-proline (152)
To a parr flask containing 2-methyl- D-proline (432 mg, 3.34 mmol, 1.0 eq.), Formaldehyde 37 wt. % in water (1.0 mL, 37 mM, 1 1 eq.), 3.5 mL of methanol and 1 mL of water, Palladium 10 wt. % on Carbon (108 mg, 0.304 mmol, 0.304 eq.) was added. The flask was placed on a parr shaker and allowed to shake under 30 psi of hydrogen for ~48 hours. Hydrogen was removed and reaction was washed through a pad of celite, which was subsequently washed with methanol. The organics where concentrated in vacuo and then azeotroped with toluene affording 152 (517 mg, 100%) as a solid. H NMR (400 MHz, methanol-^): δ [3.61-3.56 (m, 1H), 3.07-2.96 (m, 1H), 2.68 (br s, 3H), 2.34-2.22 (m, 1H), 2.01- 1.88 (m, 1H), 1.87-1.73 (m, 1H), 1.40 (br s, 3H)].
References:
WO2013/72813,2013,A2 Location in patent:Page/Page column 190
63399-77-9
154 suppliers
$30.00/250mg
1268520-34-8
8 suppliers
inquiry