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

HRID 1728196노트

반응식

HRID 1728196 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 47709505-Chloro-2-(2,2,2-trifluoroethoxy)benzaldehyde수율 838.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-07a8f31170b8417182be68635644ed4b
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07495007B2

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