Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | Malononitrile | HCID 8010 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178481140 | HCID 178481140 | — |
Reaction Steps
99 g of malononitrile were dissolved in 150 ml of N,N-dimethylformamide (DMF) and cooled to 0° C. While cooling, 556 g of tributylamine and 169.5 g of chloroacetyl chloride were simultaneously added dropwise to this, and the mixture was then stirred at 10° C. for 10 minutes. The reaction mixture was subsequently added to a mixture of 1.5 kg of ice and 327 ml of 40% by weight aqueous methylamine solution and stirred at room temperature for 8 hours. The precipitate was filtered off with suction, washed and dried in an oven at 50° C. 124 g (60% of theory) of the compound of the formula ##STR22## of melting point 300° C. were obtained. The IR, NMR, UV and mass spectra and the elemental analysis are consistent with the structural formula.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05003081 |
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| Source dataset | uspto-grants-1991_03 |
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| ORD ID | ord-a6e503c8ac3e49be8506da80e2a0f8ae |
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| Source note | uspto-grants-1991_03 |
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