4-Hydroxybenzaldehyde → HCID 59730014, 화합물

HRID 130732

반응식

HRID 130732 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[Cl:10][C:11]1[CH:18]=[C:17](F)[CH:16]=[CH:15][C:12]=1[C:13]#[N:14].C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[Cl:10][C:11]1[CH:18]=[C:17]([O:1][C:2]2[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=2)[CH:16]=[CH:15][C:12]=1[C:13]#[N:14]

참가 물질

6

반응물 4

HCID 1264-HydroxybenzaldehydeHCID 962WaterHCID 11430Potassium CarbonateHCID 1090002-Chloro-4-fluorobenzonitrile

생성물 1

HCID 59730014HCID 59730014, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-Hydroxy benzaldehyde (1 equiv), 2-chloro-4-fluorobenzonitrile (1 equiv) and K2CO3 (2.5 equiv) in anhydrous DMF (0.2 M) were heated at 110° C. under nitrogen during 1 hour (the reaction can be monitored by tlc). After cooling down to room temperature, the reaction mixture was poured into water and extracted with ethyl acetate (3×50 mL). The combined organic layer was dried over Na2SO4, filtered and concentrated under vacuum (toluene was added to aid DMF evaporation). The crude mixture was purified by flash chromatography using hexanes/ethyl acetate (4:1) as eluent.

후처리

  1. customthe reaction
  2. extractionextracted with ethyl acetate (3×50 mL)
  3. dry with materialThe combined organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum (toluene was added to aid DMF evaporation)
  6. customThe crude mixture was purified by flash chromatography

출처 및 근거

ORD 기록
ord-d284882dfca44239b0836b3ccd0b53d2
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07381719B2

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