Water → HCID 9816197, 화합물

HRID 586795노트

반응식

HRID 586795 반응식
[OH:1][CH:2]([CH3:17])[C:3]([NH:6][C:7](=[O:16])[C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[F:15])([CH3:5])[CH3:4].C(N(CC)CC)C.O>CS(C)=O>[O:1]=[C:2]([CH3:17])[C:3]([NH:6][C:7](=[O:16])[C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[F:15])([CH3:4])[CH3:5]

참가 물질

5

반응물 3

HCID 962WaterHCID 8471TriethylamineHCID 9816246HCID 9816246, 화합물

생성물 1

HCID 9816197HCID 9816197, 화합물수율 82.9%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of N-(2-hydroxy-1,1-dimethylpropyl)-2,4-difluorobenzamide obtained in Example 33 (0.30 g, 1.2 mmol) and triethylamine (0.37 g, 3.7 mmol) in DMSO (3 ml) was added pyridine sulfur trioxide complex (0.59 g, 3.7 mmol) portionwise and stirred at room temperature for 3 hours. The reaction mixture was added to a mixture of ice and water and extracted with ethyl acetate. The extract was washed with 1N hydrochloric acid, saturated aqueous NaHCO3 and brine, successively dried over Na2SO4 and concentrated under a reduced pressure. The residue was crystallized from hexane/ethyl acetate to give the title compound (0.24 g; 81%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with 1N hydrochloric acid, saturated aqueous NaHCO3 and brine
  3. dry with materialsuccessively dried over Na2SO4
  4. concentrationconcentrated under a reduced pressure
  5. customThe residue was crystallized from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-28919325596b47d9b18815170a447f56
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936736B2

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