Methylamine → N-Methyl-5-((trifluoromethyl)thio)pyridin-2-amine

HRID 1750051노트

반응식

HRID 1750051 반응식
CN.Cl[C:4]1[CH:9]=[CH:8][C:7]([S:10][C:11]([F:14])([F:13])[F:12])=[CH:6][N:5]=1.[CH3:15][N:16]1C(=O)CCC1.C(=O)([O-])[O-].[K+].[K+]>O>[CH3:15][NH:16][C:4]1[CH:9]=[CH:8][C:7]([S:10][C:11]([F:14])([F:13])[F:12])=[CH:6][N:5]=1

참가 물질

6

반응물 4

HCID 6329Methylamine2회HCID 11430Potassium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 754064102-Chloro-5-((trifluoromethyl)sulfanyl)pyridine

생성물 1

HCID 67982149N-Methyl-5-((trifluoromethyl)thio)pyridin-2-amine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

1.86 g of an aqueous methylamine solution (40%) was added dropwise to a mixture of 1.71 g of 2-chloro-5-trifluoromethylsulfanylpyridine and 16 ml of NMP, and then the mixture was heated to 60° C. and heated and stirred for 2 hours. After cooling the mixture to room temperature, 1.66 g of potassium carbonate was added, and 1.86 g of a 40% aqueous methylamine solution was added dropwise. The mixture was heated to 60° C. and further heated and stirred for 2 hours. After cooling the mixture to room temperature, water was added, and the mixture was extracted with ethyl acetate. The combined organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 1.52 g of methyl-(5-trifluoromethylsulfanylpyridin-2-yl)-amine.

후처리

  1. temperatureheated
  2. temperatureAfter cooling the mixture to room temperature
  3. temperatureThe mixture was heated to 60° C.
  4. temperaturefurther heated
  5. stirringstirred for 2 hours
  6. temperatureAfter cooling the mixture to room temperature
  7. extractionthe mixture was extracted with ethyl acetate
  8. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-333fe831be05445a90b70cd4942753b2
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156838B2

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