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Phenyl isocyanate → HCID 18674015, 화합물

HRID 1635932
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HRID 1635932 반응식
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[C:3]=1[C:15]1[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=1.[C:21]1([N:27]=[C:28]=[O:29])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.CN(C1C=CC=CN=1)C>ClCCl>[F:14][C:11]1[CH:10]=[CH:9][C:8]([C:4]2[C:3]([C:15]3[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=3)=[C:2]([NH:1][C:28]([NH:27][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[O:29])[N:6]([CH3:7])[N:5]=2)=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7672Phenyl isocyanateHCID 218852-DimethylaminopyridineHCID 18674213HCID 18674213, 화합물

생성물 1

HCID 18674015HCID 18674015, 화합물수율 32.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

150 mg of 5-amino-3-(4-fluorophenyl)-1-methyl-4-(4-pyridyl)pyrazole was dissolved in 5 ml of dichloromethane. Then, 80 mg of phenyl isocyanate and 80 mg of dimethylaminopyridine were added thereto, followed by stirring at room temperature overnight. After the reaction mixture was washed with water and dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was purified by column chromatography using 20 g of silica gel and eluted with chloroform-methanol (50:1). Thus, 70 mg of the title compound was obtained and crystallized from ether.

후처리

  1. washAfter the reaction mixture was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe resulting residue was purified by column chromatography
  5. washeluted with chloroform-methanol (50:1)

출처 및 근거

ORD 기록
ord-b152e88d2b5246c8b68f3aeddb1e972c
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06511997B1

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