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 cooled to -5° C. in an ice-methanol bath. 33 g (0.72 mol) Methylhydrazine in 100 ml ether was added dropwise so that the inner temperature did not rise above 0° C. The mixture was stirred for 1 hour at 0° C., the precipitate filtered off, washed with ether and dried in vacuo at 40° C. The intermediate was immersed for 10 minutes in an oil bath heated to 120° C. The reduction product was recrystallised from methanol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05405829 |
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| Source dataset | uspto-grants-1995_04 |
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| ORD ID | ord-748e55626fe74fea8851e6a0656a96bd |
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| Source note | uspto-grants-1995_04 |
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