Potassium Carbonate → HCID 44404786, 화합물

HRID 1976468노트

반응식

HRID 1976468 반응식
[CH3:1][O:2][C:3](=[O:25])[CH:4]([NH:10][S:11]([C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:21][C:22]#[C:23][CH3:24])=[CH:16][CH:15]=1)(=[O:13])=[O:12])[CH2:5][O:6][CH2:7][CH2:8]Br.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:21]([O:20][C:17]1[CH:18]=[CH:19][C:14]([S:11]([N:10]2[CH2:8][CH2:7][O:6][CH2:5][CH:4]2[C:3]([O:2][CH3:1])=[O:25])(=[O:13])=[O:12])=[CH:15][CH:16]=1)[C:22]#[C:23][CH3:24]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 44404785HCID 44404785, 화합물

생성물 1

HCID 44404786HCID 44404786, 화합물수율 73.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 3-(2-bromo-ethoxy)-2-(4-[2-butynyloxy]-benzenesulfonyl-amino)propionic acid methyl ester (0.15 g, 0.35 mmol) dissolved in DMF (2 mL) and cooled in an ice bath was added potassium carbonate (0.16 g, 1.15 mmol) and the reaction was stirred at room temperature for 1 hour. After removing the solvent, the residue was extracted with ethyl acetate and water. The organic layer was washed with water and brine, dried over sodium sulfate, filtered, and concentrated to give 0.09 g of 4-([4-(2-butynyloxy)phenyl]sulfonyl}-morpholine-3-carboxylic acid, methyl ester as an oil. Yield ˜73.8%. Electrospray Mass Spec 354.2 (M+H)+.

후처리

  1. temperaturecooled in an ice bath
  2. customAfter removing the solvent
  3. extractionthe residue was extracted with ethyl acetate and water
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-928e7e23be374ea4bbf45f0683e29246
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06225311B1

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