1,1-Dimethyl-2-methylenehydrazine synthesis
- Product Name:1,1-Dimethyl-2-methylenehydrazine
- CAS Number:2035-89-4
- Molecular formula:C3H8N2
- Molecular Weight:72.11
Yield:2035-89-4 77%
Reaction Conditions:
Stage #1:formaldehyd;N,N-Dimethylhydrazine for 1 h;
Stage #2: with sodium sulfate in n-heptane for 0.0833333 h;
Steps:
36
Combine dimethyl hydrazine (10.63 mL, 139.77 mmol) and paraformaldehyde(4.20 g, 0.33 eq). Stir the reaction for 1 hour. Add heptane (20 mL) and sodium sulfate (20 g). Stir 5 minutes, then filter off the sodium sulfate. Distill the filtrate with a short path distillation apparatus, collecting the title compound as a 75% w/w solution with heptane (10.3 g, 77%). ¾ NMR (400 MHz, CDC13) δ 6.10 (m, 2H), 2.80 (s, 6H).
References:
ELI LILLY AND COMPANY;BEIGHT, Douglas, Wade;BURKHOLDER, Timothy, Paul;CLAYTON, Joshua, Ryan;EGGEN, MariJean;HENRY, Kenneth, James, Junior;JOHNS, Deidre, Michelle;PARTHASARATHY, Saravanan;PEI, Huaxing;REMPALA, Mark, Edward;SAWYER, Jason, Scott WO2011/50016, 2011, A1 Location in patent:Page/Page column 38
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