1-(3-HYDROXYPROPYL)-4-METHYLPIPERAZINE synthesis
- Product Name:1-(3-HYDROXYPROPYL)-4-METHYLPIPERAZINE
- CAS Number:5317-33-9
- Molecular formula:C8H18N2O
- Molecular Weight:158.24
Yield:5317-33-9 86%
Reaction Conditions:
in toluene at 80;
Steps:
Intermediate 7: 3-(4-Methylpiperazin-1-yl)-propan-1-ol.
Intermediate 7: 3-(4-Methylpiperazin-1-yl)-propan-1-ol. 1-Methylpiperazine (6.99 mL, 63 mol) was dissolved in toluene (30 mL). 3-Bromo-propanol (2.62 mL, 30 mmol) was added slowly and the mixture was stirred overnight. After heating to 80°C for 2 h and cooling to r.t., the mixture was filtered and the filter cake was washed thoroughly with toluene. After removal of the toluene, the residue was subjected to Kugelrohr distillation (b.p., 180°C / 2 mbar) to obtain a colourless oil (4.08 g, 25.8 mmol, 86 %). 1H NMR (CDCl3): δ = 1.70 (Ψ-quint, J ≈ 5.8 Hz, 2 H), 2.26 (s, 3 H), 2.35-2.6 (m, 8 H), 2.60 (Ψ-t, J = 5.8 Hz, 2 H), 3.77 (Ψ-t, J = 5.3 Hz, 2 H), 4.09 (s, br., 1 H).
References:
4SC AG EP1674467, 2006, A1 Location in patent:Page/Page column 26
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