反应详情

温度

50 °C

LiAlH4 (1M in THF, 47 mL, 47 mmol, 1.5 equiv) was added to a solution of 3,3,4-trimethyl-piperazin-2-one (Step 107.3) (4.5 g, 32 mmol) in THF (50 mL) at 50° C., under an argon atmosphere. The resulting mixture was stirred for 2 h at 50° C., quenched by addition of acetone, filtered through a pad of celite and concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 94:5:1) to afford 1.9 g of the title compound as a yellow oil. Title compound: ESI-MS: 129.1 [M+H]+.

1. customquenched by addition of acetone
2. filtrationfiltered through a pad of celite
3. concentrationconcentrated
4. customThe residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 94:5:1)