Potassium Carbonate → 5-Chloro-2-(2,2,2-trifluoroethoxy)benzaldehyde

HRID 1728196ノート

反応式

HRID 1728196 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].[F:11][C:12]([F:16])([F:15])[CH2:13]I.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:10][CH2:13][C:12]([F:16])([F:15])[F:11])=[C:6]([CH:9]=1)[CH:7]=[O:8]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 124815-Chloro-salicylaldehydeHCID 677091,1,1-Trifluoro-2-iodoethane

生成物 1

HCID 47709505-Chloro-2-(2,2,2-trifluoroethoxy)benzaldehyde収率 838.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5-Chloro-2-hydroxy-benzaldehyde (3.1 g, 2 mmol), 1,1,1-trifluoro-2-iodo-ethane (2.4 mL, 24 mmol), K2CO3 (5.5 g, 40 mmol) and KI (0.1 g) were mixed in DMF (20 mL). Then the mixture was irradiated under microwave at 180° C. for 1 h. The mixture was filtered and the filtrate was concentrated. The residue was dissolved in ethyl acetate and washed with 1N NaOH. Then the organic layer was separated, dried over anhydrous Na2SO4 and concentrated to give title compound as a yellow solid (Yield: 4 g).

後処理

  1. customThen the mixture was irradiated under microwave at 180° C. for 1 h
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with 1N NaOH
  6. customThen the organic layer was separated
  7. dry with materialdried over anhydrous Na2SO4
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-07a8f31170b8417182be68635644ed4b
出典データセット
uspto-grants-2009_02
特許番号
US07495007B2

反応ノート

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