Potassium Carbonate → 5-Chloro-2-(3-hydroxy-propoxy)-benzaldehyde

HRID 1728201

반응식

HRID 1728201 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].Br[CH2:12][CH2:13][CH2:14][OH:15].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:10][CH2:12][CH2:13][CH2:14][OH:15])=[C:6]([CH:9]=1)[CH:7]=[O:8]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 123083-Bromo-1-propanolHCID 124815-Chloro-salicylaldehyde

생성물 1

HCID 575659355-Chloro-2-(3-hydroxy-propoxy)-benzaldehyde수율 59%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5-Chloro-2-hydroxy-benzaldehyde (3.1 g, 20 mmol), 3-bromo-propan-1-ol (4.1 mL, 24 mmol), K2CO3 (5.5 g, 4 mmol) and KI (0.5 g) were mixed in DMF (20 mL). Then the mixture was irradiated under microwave at 200° 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 Na2SO4 and concentrated to give title compound (Yield: 1.7 g, 59%).

후처리

  1. customThen the mixture was irradiated under microwave at 200° 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 Na2SO4
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-653dbb65be664e1fbbcc871c9d5ff7d6
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07495007B2

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