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Water → HCID 15540300, 화합물

HRID 393143
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HRID 393143 반응식
[F:1][C:2]([F:16])([F:15])[C:3]1[C:8]([CH:9]([NH:13][CH3:14])[CH:10]([CH3:12])[CH3:11])=[CH:7][N:6]=[CH:5][N:4]=1.C(=O)([O-])[O-].[K+].[K+].[C:23]1([CH2:29][C:30](Cl)=[O:31])[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.O>C(#N)C>[CH3:14][N:13]([CH:9]([C:8]1[C:3]([C:2]([F:1])([F:15])[F:16])=[N:4][CH:5]=[N:6][CH:7]=1)[CH:10]([CH3:12])[CH3:11])[C:30](=[O:31])[CH2:29][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 7679Phenylacetyl chlorideHCID 11430Potassium CarbonateHCID 22648743HCID 22648743, 화합물

생성물 1

HCID 15540300HCID 15540300, 화합물수율 85%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

6 g (26 mmol) of 4-trifluoromethyl-5-[1-(N-methylamino)-2-methylpropyl]pyrimidine and 3.6 g (26 mmol) of potassium carbonate were dissolved in 150 ml of acetonitrile, and 4 g (26 mmol) of phenylacetyl chloride was dropwise added, followed by stirring at room temperature for 3 hours. To the reaction solution, 200 ml of water was added, followed by extraction with ethyl acetate. The obtained organic layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and the obtained crude crystals were washed with n-hexane to obtain 7.7 g (yield: 85%) of N-methyl-N-[2-methyl-1-(4-trifluoromethylpyrimidin-5-yl)propyl]phenylacetamide as colorless transparent crystals (melting point: 106-109° C.).

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe obtained organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationEthyl acetate was distilled off under reduced pressure
  5. customthe obtained crude crystals
  6. washwere washed with n-hexane

출처 및 근거

ORD 기록
ord-0e1f101c4adf4ddcbc3652a2021644cd
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06806230B1

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