methyl 4-methylpiperazine-1-carboxylate synthesis
- Product Name:methyl 4-methylpiperazine-1-carboxylate
- CAS Number:7560-85-2
- Molecular formula:C7H14N2O2
- Molecular Weight:158.2
Yield:7560-85-2 82.5%
Reaction Conditions:
with sodium cyanide in dichloromethane at 0 - 20; for 2 h;
Steps:
1 Example 1: The preparation method of methyl 4-methylpiperazine-1-carboxylate
1. Add 10 g of 4-methylpiperazine-1-formyl chloride hydrochloride and 50 ml of dichloromethane into the reaction flask, then add 5 ml of methanol, then cool down to 0-5°C, add 2 g of sodium cyanide in batches, return to room temperature and stir for 2 hours after the addition.2. After adding water (50ml) to the system, adjust the pH to 6.4 with 4M dilute hydrochloric acid, stir at room temperature, separate the liquid, and keep the water phase.3. The aqueous phase was adjusted to pH 9 with an aqueous sodium carbonate solution, extracted twice with 50 ml of dichloromethane, the organic phases were combined and dried, and the organic phase was spin-dried at 40°C in vacuo to obtain 6.6 g of methyl 4-methylpiperazine-1-carboxylate as a light yellow transparent oil. The yield was 82.5%, and the purity was 98.3%.
References:
CN114763342,2022,A Location in patent:Paragraph 0050-0055
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