Sodium Cyanide → HCID 14461236, 화합물

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Cl[CH2:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.[C-:20]#[N:21].[Na+]>O.C(O)C>[C:20]([CH2:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1)#[N:21]

참가 물질

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온도: 80 °C

실험 절차

In a 50 ml round-bottom two-necked flask, 2.0 g were suspended in 2.0 ml of water and heated to 80° C. A 9.2 g amount of 4-(4'-chloromethylbenzyl)benzotrifluoride was dissolved in 7.1 ml of ethanol. This solution was added dropwise into the NaCN suspension. The proportion of undissolved substances increased. The reaction mixture turned brown. The feedstock was boiled under reflux for 5 hours. After the reaction mixture had cooled down to room temperature, the solid substance was removed by filtration and washed with 30 ml ethanol. The filtration was concentrated in a rotary evaporator (bath temp. 30° C., water-jet vacuum). The oily residue was dissolved in 50 ml of diethyl ether and washed to neutrality four times with 30 ml of water each time. The organic phase was dried over sodium sulfate. The drying agent was removed by filtration and the ether was removed by distillation in a rotary evaporator (bath temp. 30° C., water-jet vacuum). The raw product (8.0 g) was chromatographed on silica gel 60 (0.63-0.200) with ether/pentane (1/4) and the 4-(4'-cyanomethylbenzyl)benzotrifluoride (5.8 g) thus obtained was recrystallized from 44 ml of solvent blend (petroleum benzin 60°-80°C0-diethyl ether 5:1 v/v). The precipitated crystallizate was removed by filtration via a D-4 glass suction funnel and washed with 25 ml of ice-cold petroleum benzin. The product was dried in a vacuum drying oven (oil pump) at room temperature for 5 hours.