Potassium Carbonate → HCID 4604295, 화합물

HRID 1521814노트

반응식

HRID 1521814 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[SH:9].C(=O)([O-])[O-].[K+].[K+].Br[CH:17]([CH3:21])[C:18]([OH:20])=[O:19]>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][CH2:21][CH2:17][C:18]([OH:20])=[O:19]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 117292-Bromopropionic acidHCID 23642Thioguaiacol

생성물 1

HCID 4604295HCID 4604295, 화합물수율 754.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-methoxythiophenol (5.0 g, 3.56 mmol) in DMF (125 mL) is added potassium carbonate (14.76 g, 10.69 mmol, 3 Eq) at 60° C. under nitrogen. The reaction mixture is stirred for 30 minutes then bromopropionic acid (6.0 g, 3.92 mmol, 1.1 Eq) is added and the resulting mixture is stirred for 90 minutes at 60° C. under nitrogen. The solvent is removed under reduced pressure and the residue is taken up in water then washed with EtOAc. The aqueous layer is acidified with aq. solution of HCl and the product is extracted with EtOAc. The organic layer is dried over MgSO4 and concentrated in under reduced pressure to afford 5.7 g (75%) of the title compound as a yellow oil.

후처리

  1. stirringthe resulting mixture is stirred for 90 minutes at 60° C. under nitrogen
  2. customThe solvent is removed under reduced pressure
  3. washthen washed with EtOAc
  4. extractionthe product is extracted with EtOAc
  5. dry with materialThe organic layer is dried over MgSO4
  6. concentrationconcentrated in under reduced pressure

출처 및 근거

ORD 기록
ord-08431bae44924cc79ef791d35f6b1ece
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073940B2

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