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Water → 1-(3,5-Difluoropyridin-2-yl)-2-(2-fluorophenyl)ethanone

HRID 570516
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HRID 570516 반응식
[F:1][C:2]1[C:3]([C:9](=[O:22])[CH:10]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[F:21])C(OC)=O)=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1.[Cl-].[Na+].O>CS(C)=O.C(OCC)(=O)C>[F:1][C:2]1[C:3]([C:9](=[O:22])[CH2:10][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[F:21])=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 5234Sodium ChlorideHCID 66635086Methyl 3-(3,5-difluoropyridin-2-yl)-2-(2-fluorophenyl)-3-oxopropanoate

생성물 1

HCID 666355431-(3,5-Difluoropyridin-2-yl)-2-(2-fluorophenyl)ethanone

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8857Ethyl Acetate
용매

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온도
150 °C

실험 절차

11.65 g (37.67 mmol) of the compound from Example 13A were initially charged in DMSO (37 ml). Subsequently, 2.42 g (41.44 mmol) of sodium chloride and water (7 ml) were added, and the mixture was stirred in a microwave at 150° C. for 30 min. The reaction mixture was diluted with ethyl acetate, and the organic phase was washed three times with water and once with saturated aqueous sodium chloride solution, dried over sodium sulphate, filtered and concentrated. This gave 9.07 g (89%, 85% of theory) of the desired compound in solid form, which was converted without further purification.

후처리

  1. washthe organic phase was washed three times with water
  2. dry with materialonce with saturated aqueous sodium chloride solution, dried over sodium sulphate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThis gave 9.07 g (89%, 85% of theory) of the desired compound in solid form, which was converted without further purification

출처 및 근거

ORD 기록
ord-88923dcd69e64635abe555c3cc4baaa8
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09023849B2

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