Dimethylformamide → 3-Amino-2-chloro-4-methyl-6-(2,2,2-trifluoro-1-trifluoromethylethoxy)pyridine

HRID 1696963노트

반응식

HRID 1696963 반응식
[NH2:1][C:2]1[C:3]([CH3:18])=[CH:4][C:5]([O:8][CH:9]([C:14]([F:17])([F:16])[F:15])[C:10]([F:13])([F:12])[F:11])=[N:6][CH:7]=1.CN(C)C=O.[Cl:24]N1C(=O)CCC1=O>O>[NH2:1][C:2]1[C:7]([Cl:24])=[N:6][C:5]([O:8][CH:9]([C:10]([F:11])([F:12])[F:13])[C:14]([F:17])([F:15])[F:16])=[CH:4][C:3]=1[CH3:18]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 31398ChlorosuccinimideHCID 860624455-Amino-4-methyl-2-(2,2,2-trifluoro-1-trifluoromethylethoxy)pyridine

생성물 1

HCID 231500063-Amino-2-chloro-4-methyl-6-(2,2,2-trifluoro-1-trifluoromethylethoxy)pyridine수율 44.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.0 g of 5-amino-4-methyl-2-(2,2,2-trifluoro-1-trifluoromethylethoxy)pyridine was introduced to 10 ml of N,N-dimethylformamide, and 0.56 g of N-chlorosuccinic acid imide was added thereto at room temperature. The resulting solution was heated to 60 degree centigrade, stirred for 1 hour, and then poured into water and extracted with ethyl acetate. The solution was dried over anhydrous magnesium sulfate, and then the solvent was removed under a reduced pressure to obtain a residue. The resulting residue was purified by silica gel column chromatography using an eluent (development solvent; hexane:ethyl acetate=10:1) to obtain 0.50 g of the desired product (Yield: 44%) as brown oil.

후처리

  1. additionwas added
  2. customat room temperature
  3. temperatureThe resulting solution was heated to 60 degree centigrade
  4. extractionextracted with ethyl acetate
  5. dry with materialThe solution was dried over anhydrous magnesium sulfate
  6. customthe solvent was removed under a reduced pressure
  7. customto obtain a residue
  8. customThe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-53dbf46c531f4f47aa1a8c0f5831feb3
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163804B2

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