Cesium carbonate → Ethyl 2-(4-(1-(((4-(trifluoromethyl)benzyl)oxy)imino)propyl)phenoxy)acetate

HRID 68307ノート

反応式

HRID 68307 の反応式
[OH:1][N:2]=[C:3]([C:6]1[CH:18]=[CH:17][C:9]([O:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:8][CH:7]=1)[CH2:4][CH3:5].C(=O)([O-])[O-].[Cs+].[Cs+].[F:25][C:26]([F:36])([F:35])[C:27]1[CH:34]=[CH:33][C:30]([CH2:31]Br)=[CH:29][CH:28]=1>CN(C=O)C>[F:25][C:26]([F:35])([F:36])[C:27]1[CH:34]=[CH:33][C:30]([CH2:31][O:1][N:2]=[C:3]([C:6]2[CH:18]=[CH:17][C:9]([O:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:8][CH:7]=2)[CH2:4][CH3:5])=[CH:29][CH:28]=1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 1230621-(Bromomethyl)-4-(trifluoromethyl)benzeneHCID 86699619Ethyl 2-(4-(1-(hydroxyimino)propyl)phenoxy)acetate

生成物 1

HCID 74371516Ethyl 2-(4-(1-(((4-(trifluoromethyl)benzyl)oxy)imino)propyl)phenoxy)acetate収率 95%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of the product of step 2 (18 g, 0.0723 moles) in DMF (54 mL), cesium carbonate (47 gm, 0.1446 moles) and 4-(trifluoromethyl)benzyl bromide (19 gm, 0.0795 moles) were added and the reaction mixture was srirred at 25° C. for 3 hours. The reaction mixture was poured into ice cold water and extracted with ethyl acetate. The combined ethyl acetate extract was washed with water & brine, dried over sodium sulphate and evapourated under reduced pressure to yield 28 gm (95%) of product as thick liquid.

後処理

  1. additionThe reaction mixture was poured into ice cold water
  2. extractionextracted with ethyl acetate
  3. extractionThe combined ethyl acetate extract
  4. washwas washed with water & brine
  5. dry with materialdried over sodium sulphate

出典と根拠

ORDレコード
ord-3d21a13bf6554cea9178ad766188e142
出典データセット
uspto-grants-2014_09
特許番号
US08822414B2

反応ノート

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