Methylamine → 3-Diphenylmethoxy-1-methylazetidine
反応式
Cl[CH2:2][CH:3]([O:6][CH:7]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH2:4]Cl.[CH3:20][NH2:21]>>[C:8]1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[O:6][CH:3]2[CH2:4][N:21]([CH3:20])[CH2:2]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1参加物
3
実験手順
A solution of 244. g (0.83 mole) of 1,3-dichloro-2-diphenylmethoxypropane in 300 ml of methylamine was heated in a steel bomb to 100° for 18 hours. The mixture was concentrated, and the residue partitioned between chloroform and dilute hydrochloric acid. The acid solution was washed twice with chloroform, and the chloroform solutions combined. The chloroform was extracted with dilute sodium hydroxide, dried with sodium sulfate, and concentrated. The residue was distilled (b.p. 125°-130°/0.1 mm) to yield 104 g (40%). The distillate crystallizes on standing and can be recrystallized from isooctane, mp 44°-48°.
後処理
- concentrationThe mixture was concentrated
- customthe residue partitioned between chloroform and dilute hydrochloric acid
- washThe acid solution was washed twice with chloroform