Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylhydrazine | HCID 6061 | — |
| Reactant | Dimethyl acetylenedicarboxylate | HCID 12980 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 178498595 | HCID 178498595 | — |
Reaction Steps
102.3 g (0.72 mol) Dimethyl acetylenedicarboxylate was added to 1000 ml ether and the mixture cooled to -5° C. in an ice-methanol bath. 33 g (0.72 mol) methylhydrazine in 100 ml ether was added dropwise at a rate that the inner temperature did not rise above 0° C. The mixture was stirred for one hour at 0° C., the precipitate suction filtered off, washed with ether and dried at 40° C. in vacuo. The intermediate was immersed in an oil-bath heated to 120° C. The reaction product was recrystallised from methanol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05756424 |
|---|
| Source dataset | uspto-grants-1998_05 |
|---|
| ORD ID | ord-9cae835384be45b6a774317b0e99d433 |
|---|
| Source note | uspto-grants-1998_05 |
|---|