壬二酰氯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 10.5 grams of azeloylchloride were placed in a container holding 140 milliliters of tetrachloroethylene and dissolved. To the resulting mixture were added 9.2 grams of N-methyl-N-hexylamine, and 1.6 grams of NaOH dissolved in 200 milliliters of water. The completed mixture was agitated for 10-15 minutes; afterwards the organic layer was separated, washed with a dilute aqueous HCl solution. Following this the organic layer was washed with a 10% aqueous Na2CO3 solution and then washed with water. The washed organic layer was dried by contacting with MgSO4 and then the tetrachloroethylene was removed by application of a vacuum. dissolved afterwards the organic layer was separated washed with a dilute aqueous HCl solution was washed with a 10% aqueous Na2CO3 solution washed with water The washed organic layer was dried the tetrachloroethylene was removed by application of a vacuum

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Thioanisole (23.5 ml, 0.20 mol) is added to a suspension of AlCl3 (27.3 g, 0.205 mol) in 200 ml of CH2Cl2. Azelaoyl chloride (19.7 ml, 0.10 mol) is added dropwise slowly, while the reaction mixture is cooled in an ice bath and the reaction solution is stirred for 19 h at room temperature. Then, the reaction solution is poured into ice-water. The produced white precipitate is filtered off and the crude product is extracted from the filtrate with CH2Cl2, washed with brine, dried over MgSO4, and concentrated. The residue is purified by recrystallization from i-Pr2O—CHCl3. The product is obtained as a white solid. 1H NMR (CDCl3), δ[ppm]: δ1.35-1.43 (m, 6H), 1.72 (t, 4H), 2.52 (s, 6H), 2.91 (t, 4H), 7.26 (d, 4H), 7.87 (d, 4H) is cooled in an ice bath The produced white precipitate is filtered off the crude product is extracted from the filtrate with CH2Cl2 washed with brine dried over MgSO4 concentrated The residue is purified by recrystallization from i-Pr2O—CHCl3 The product is obtained as a white solid