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Water → HCID 70692250, 화합물

HRID 576740
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HRID 576740 반응식
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([NH:9][CH2:10][CH2:11][C:12]([OH:14])=O)[CH:6]=[CH:7][CH:8]=1.[NH2:17][C:18](N)=[O:19].O>C(O)(=O)C>[F:15][C:2]([F:1])([F:16])[C:3]1[CH:4]=[C:5]([N:9]2[CH2:10][CH2:11][C:12](=[O:14])[NH:17][C:18]2=[O:19])[CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 1176UreaHCID 172449643-(3-Trifluoromethylphenylamino)propionic acid

생성물 1

HCID 70692250HCID 70692250, 화합물수율 67.7%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 3-(3-trifluoromethylphenylamino)propanoic acid (2.0 g) (prepared in Reference Example 95) and urea (1.0 g) in acetic acid (20.0 ml) was stirred with heating under reflux for seven hours. To the reaction mixture was water (50 ml) and the resulting mixture was extracted with ethyl acetate (30 ml×3). The organic layer was washed with water (20 ml×2) and saturated saline (20 ml), dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol) to afford 1-(3-trifluoromethylphenyl)dihydropyrimidin-2,4(1H,3H)-dione (1.5 g).

후처리

  1. temperaturewith heating
  2. temperatureunder reflux for seven hours
  3. extractionthe resulting mixture was extracted with ethyl acetate (30 ml×3)
  4. washThe organic layer was washed with water (20 ml×2) and saturated saline (20 ml)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol)

출처 및 근거

ORD 기록
ord-01e4fb164a7046e0a71844c037b83308
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040516B2

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