1,2-Benzenedimethanol → N,N-Diisopropyl-1,5-dihydrobenzo[e][1,3,2]dioxaphosphepin-3-amine
反応式
[OH:1][CH2:2][C:3]1[C:4](=[CH:7][CH:8]=[CH:9][CH:10]=1)[CH2:5][OH:6].[CH:11]([N:14]([P:18](N(C(C)C)C(C)C)Cl)[CH:15]([CH3:17])[CH3:16])([CH3:13])[CH3:12]>C1COCC1>[CH:11]([N:14]([CH:15]([CH3:17])[CH3:16])[P:18]1[O:6][CH2:5][C:4]2[CH:7]=[CH:8][CH:9]=[CH:10][C:3]=2[CH2:2][O:1]1)([CH3:13])[CH3:12]参加物
4
実験手順
Phthalyl alcohol (1.15 g, 8.31 mmol) was dissolved in 5 ml of THF, and bisdiisopropylaminochlorophosphine (2.21 g, 8.31 mmol) which was dissolved in 5 ml of THF was added dropwise to the solution at -15° C. under a nitrogen atmosphere. Afterward, the temperature of the solution was adjusted to room temperature, and after the disappearance of phthalyl alcohol had been confirmed, hydrochloride of diisopropylamine was washed with ether. The wash liquor was concentrated and then distilled in order to obtain the desired product having a melting point of from 150° to 155° C. (0.7 mmHg).