Ammonia → 2-Amino-2,4-dimethylpentanenitrile
Reaction equation
[NH3:1].O[C:3]([CH3:10])([CH2:6][CH:7]([CH3:9])[CH3:8])[C:4]#[N:5]>O>[NH2:1][C:3]([CH3:10])([CH2:6][CH:7]([CH3:9])[CH3:8])[C:4]#[N:5]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a 1-liter autoclave were added 7 moles of ammonia and then 3.5 moles of 90%-pure 2-hydroxy-2,4-dimethylpentanonitrile, and the mixture was reacted at 27° C. for 10 hours at a rate of 300 r.p.m. Thus, 2-amino-2,4-dimethylpentanonitrile was synthesized. After reaction, the reaction mixture was taken out of the autoclave, and 44 g of the water phase was separated. The residue was distilled in a wetted wall tower under the following conditions: Temperature of the heating portion 25° C.; pressure 30 mmHg; and residence time in the heating portion 1 minute or less. Low-boiling compounds were thus distilled off and purified 2-amino-2,4-dimethylpentanonitrile was withdrawn from the bottom. The yield of the purified product was 90.0 mole % based on cyanohydrin. This purified product contained 0.5% by weight of ammonia and 0.8% by weight of hydrogen cyanide, and its purity was 90%.
Workup
- customAfter reaction
- customwas separated
- distillationThe residue was distilled in a wetted wall tower under the following conditions
- customTemperature of the heating portion 25° C.
- customin the heating portion 1 minute or less
- distillationwere thus distilled off
- custompurified 2-amino-2,4-dimethylpentanonitrile
- customwas withdrawn from the bottom
Sources & evidence
- ORD record
- ord-b8876ba487894cda80e0fd7f7c84600d
- Source dataset
- uspto-grants-1981_06
- Patent number
- US04272435
Reaction notes
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