Potassium Iodide → Triethyl 2-[4-(trifluoromethoxy)phenyl]ethane-1,1,1-tricarboxylate

HRID 1256884

반응식

HRID 1256884 반응식
[CH:1]([C:12]([O:14][CH2:15][CH3:16])=[O:13])([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:2]([O:4][CH2:5][CH3:6])=[O:3].[F:17][C:18]([F:29])([F:28])[O:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24]Br)=[CH:22][CH:21]=1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O.C(OCC)(=O)C>[F:17][C:18]([F:28])([F:29])[O:19][C:20]1[CH:21]=[CH:22][C:23]([CH2:24][C:1]([C:12]([O:14][CH2:15][CH3:16])=[O:13])([C:2]([O:4][CH2:5][CH3:6])=[O:3])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:26][CH:27]=1

참가 물질

8

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 80471Triethyl methanetricarboxylateHCID 1427851-(Bromomethyl)-4-(trifluoromethoxy)benzene

생성물 1

HCID 68511908Triethyl 2-[4-(trifluoromethoxy)phenyl]ethane-1,1,1-tricarboxylate수율 100.1%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of triethyl methanetricarboxylate (4.55 g) in DMF (40 mL) were added 4-(trifluoromethoxy)benzyl bromide (5.00 g), potassium iodide in catalytic amount and potassium carbonate (4.07 g), and the mixture was stirred at room temperature for 3 hr. Ethyl acetate (200 mL) and water (100 mL) were added to extract the reaction mixture. The extract was washed sequentially with water and brine, and concentrated under reduced pressure to give the title compound (7.97 g) as an oil.

후처리

  1. extractionto extract the reaction mixture
  2. washThe extract was washed sequentially with water and brine
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f801f66264d84429acaf4c1228a48aaa
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461209B2

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