Methanol → HCID 23282353、化合物

反応式

[CH2:1]([C:3]1[CH:17]=[C:16]([O:18][CH2:19][CH:20]=[C:21]([Cl:23])[Cl:22])[CH:15]=[C:14]([CH2:24][CH3:25])[C:4]=1[O:5][CH2:6][CH2:7][CH2:8][CH2:9][O:10][CH2:11][CH:12]=[O:13])[CH3:2].[Cl-].[NH4+].[C:28](=[O:31])([O-])O.[Na+].[CH3:33]O>>[CH2:24]([C:14]1[CH:15]=[C:16]([O:18][CH2:19][CH:20]=[C:21]([Cl:22])[Cl:23])[CH:17]=[C:3]([CH2:1][CH3:2])[C:4]=1[O:5][CH2:6][CH2:7][CH2:8][CH2:9][O:10][CH2:11][CH:12]([O:31][CH3:28])[O:13][CH3:33])[CH3:25]

参加物

反応物 4

HCID 887Methanol

HCID 25517Ammonium Chloride

HCID 516892Sodium Bicarbonate

HCID 54234953HCID 54234953、化合物

生成物 1

HCID 23282353HCID 23282353、化合物収率 71%

実験手順

First, 0.39 g of 4-(2,6-diethyl-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde was dissolved in 10 ml of anhydrous methanol, to which 5 mg of ammonium chloride was added, and the mixture was heated under reflux for 3 hours After left alone for cooling, the reaction mixture was mixed with 10 ml of saturated aqueous sodium hydrogencarbonate solution. The methanol was distilled out, and the residue was extracted twice with diethyl ether. The diethyl ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and then concentrated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 0.31 g of 3,5-diethyl-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-dimethoxyethoxy)butyloxy)benzene (yield, 71%), nD24.0 1.5068.