Triethylamine → 1-n-Hexadecyloxycarbonyloxy-1-methyl-2-acetylethene

HRID 1252515

반응식

HRID 1252515 반응식
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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31261AcetylacetoneHCID 97633Cetyl chloroformate

생성물 1

HCID 543845731-n-Hexadecyloxycarbonyloxy-1-methyl-2-acetylethene

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  1. waitto stand for 2 days
  2. customThe precipitate is isolated by filtration
  3. washwashed with diethyl ether
  4. washThe filtrate is washed twice with water
  5. dry with materialdried over Na2SO4
  6. concentrationFirst the solution is concentrated by rotary evaporation
  7. distillationthe residual acetylacetone and the dietyl ether are distilled off with an oil pump
  8. customto give colourless crystals with a melting point of 33°-35° C.

출처 및 근거

ORD 기록
ord-6721c8bbdf784479a4b879373692b456
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04743640

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