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ChemicalBook CAS DataBase List 3-amino-2-methylpropan-1-ol

3-amino-2-methylpropan-1-ol synthesis

4synthesis methods
-

Yield: 86%

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran at 0; for 3 h;Inert atmosphere;Reflux;

Steps:

2 Synthesis of aminoalcohol (D2).
D1 (2.0 g, 13.0 mmol) was added portionwise to a suspension of LiAIH4 (1.4 g, 39.2 mmol) in THF (75 ml_) under nitrogen atmosphere at 0 °C. The reaction mixture was stirred for 30 minutes and then allowed to stir at room temperature for another 30 minutes. The reaction mixture was refluxed for 2 h, and then it was cooled to -10 °C and quenched carefully with ice cold water (1.4 ml_). 10% NaOH solution (2.8 ml_) and ice cold water (4.2 ml_) were added, and the mixture was stirred for 15 minutes. It was filtered, and the filtrate washed with EtOAc (3 x 100 ml_), dried over anhydrous Na2S04 and concentrated under vacuum to obtain D2 (1.2 g, 86%) as a pale yellow liquid. Rf: 0.2 (20% MeOH in DCM). 1H NMR (400 MHz, cf6-DMSO): δ 0.78 (d, J = 6.8 Hz, 3H), 1.46 - 1.54 (m, 1 H), 2.41 - 2.45 (m, 2H), 2.50 - 2.54 (m, 1 H), 3.22 - 3.34 (m, 4H).

References:

Location in patent:Page/Page column 142

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