反応式
Cl[C:2]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])=[O:3].[C:21]([CH2:24][C:25](=[O:27])[CH3:26])(=[O:23])[CH3:22].C(N(CC)CC)C>C(OCC)C>[CH2:5]([O:4][C:2]([O:27][C:25]([CH3:26])=[CH:24][C:21](=[O:23])[CH3:22])=[O:3])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]参加物
実験手順
30.4 g (0.1 mole) of n-hexadecyl chloroformate, 15 g (0.15 mole) of acetylacetone and 80 ml of diethyl ether are charged to a 250 ml flask. Then a solution of 11 g (0.11 mole) of triethylamine in 20 ml of diethyl ether is added, with stirring, at a temperature below 10° C. over 25 minutes. The mixture is warmed to room temperature and allowed to stand for 2 days. The precipitate is isolated by filtration and washed with diethyl ether. The residue is triethylamine hydrochloride (13.8 g; theory: 13.8 g). The filtrate is washed twice with water and then dried over Na2SO4. First the solution is concentrated by rotary evaporation and then the residual acetylacetone and the dietyl ether are distilled off with an oil pump, to give colourless crystals with a melting point of 33°-35° C.
後処理
- waitto stand for 2 days
- customThe precipitate is isolated by filtration
- washwashed with diethyl ether
- washThe filtrate is washed twice with water
- dry with materialdried over Na2SO4
- concentrationFirst the solution is concentrated by rotary evaporation
- distillationthe residual acetylacetone and the dietyl ether are distilled off with an oil pump
- customto give colourless crystals with a melting point of 33°-35° C.
出典と根拠
- ORDレコード
- ord-6721c8bbdf784479a4b879373692b456
- 出典データセット
- uspto-grants-1988_05
- 特許番号
- US04743640
関連ノート
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