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

HRID 1256884

反応式

HRID 1256884 の反応式
[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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f801f66264d84429acaf4c1228a48aaa
出典データセット
uspto-grants-2013_06
特許番号
US08461209B2

関連ノート

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