Triethylamine → HCID 54343021, 화합물

HRID 1872397

반응식

HRID 1872397 반응식
[C:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[CH2:15]([O:20][C:21]1[CH:28]=[CH:27][C:24]([CH:25]=O)=[CH:23][CH:22]=1)[CH2:16][CH2:17][CH2:18][CH3:19].C(N(CC)CC)C>ClCCl.C(OCC)(=O)C.[Ti](Cl)(Cl)(Cl)Cl>[CH2:15]([O:20][C:21]1[CH:28]=[CH:27][C:24]([CH:25]=[CH:2][C:1]([C:4]2[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=2)=[O:3])=[CH:23][CH:22]=1)[CH2:16][CH2:17][CH2:18][CH3:19]

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 79815p-PentoxybenzaldehydeHCID 600911Ethyl 4-acetylbenzoate

생성물 1

HCID 54343021HCID 54343021, 화합물수율 61.2%

시약·촉매·용매 3

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매3회HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

To a solution of titanium(IV) chloride (13.88 g) in dichloromethane (100 ml) was added Ethyl 4-acetylbenzoate (11.53 g) and 4-n-pentyloxybenzaldehyde (12.68 g) in dichloromethane (50 ml) was added dropwise at 0° C. To the mixture was added triethylamine (12.44 ml) in dichloromethane (30 ml). The mixture was stirred at 0° C. for 30 minutes and diluted with ethyl acetate. The organic layer was washed with water (four times) and brine and dried over magnesium sulfate. The solvents were removed under reduced pressure and the residue was triturated with n-hexane. The solid was collected by filtration and dried to give 1-(4-n-Pentyloxyphenyl)-3-(4-ethoxycarbonylphenyl)-1-propen-3-one (13.45 g).

후처리

  1. additionwas added dropwise at 0° C
  2. washThe organic layer was washed with water (four times) and brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvents were removed under reduced pressure
  5. customthe residue was triturated with n-hexane
  6. filtrationThe solid was collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-5929b187f2df40f981646c2892dd1128
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107458

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