Isopropylamine → HCID 178456414, compound
Reaction equation
[C:1](#[N:5])[CH2:2][C:3]#[N:4].C(N(CC)CC)C.Cl[CH2:14][C:15](Cl)=[O:16].[CH:18]([NH2:21])([CH3:20])[CH3:19]>CN(C=O)C>[NH2:4][C:3]1[N:21]([CH:18]([CH3:20])[CH3:19])[CH2:14][C:15](=[O:16])[C:2]=1[C:1]#[N:5]Participants
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
99 g of malononitrile were dissolved in 150 ml of DMF and cooled to 0° C. While cooling, 306 g of triethylamine and 159 g of chloroacetyl chloride were simultaneously added dropwise to this. The reaction mixture was stirred at 10° C. for 10 minutes and subsequently added to a mixture of 1.5 kg of ice and 158 g of isopropylamine. The mixture was stirred at room temperature for 8 hours. The volatiles were then removed by distillation under atmospheric pressure at 100° C., and the distillation residue was cooled to 5° C. The precipitate was filtered off with suction, washed and dried. 105.6 g (43% of theory) of the compound of the formula ##STR24## of melting point 285° to 290° C. were obtained. The IR, NMR, UV and mass spectra and the elemental analysis are consistent with the structural formula.
Workup
- temperatureWhile cooling
- stirringThe mixture was stirred at room temperature for 8 hours
- customThe volatiles were then removed by distillation under atmospheric pressure at 100° C.
- temperaturethe distillation residue was cooled to 5° C
- filtrationThe precipitate was filtered off with suction
- washwashed
- customdried
- custom105.6 g (43% of theory) of the compound of the formula ##STR24## of melting point 285° to 290° C. were obtained
Sources & evidence
- ORD record
- ord-3b758ac156644b9aad428d4fbc3ec8c8
- Source dataset
- uspto-grants-1991_03
- Patent number
- US05003081
Reaction notes
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