1,2-Dichloroethane → HCID 118020438, 화합물

HRID 1747511노트

반응식

HRID 1747511 반응식
C(Cl)CCl.[CH3:5][NH:6][CH3:7].[Cl:8][C:9]1[N:14]=[C:13]([C:15](O)=[O:16])[C:12]([C:18]([F:21])([F:20])[F:19])=[CH:11][CH:10]=1.[Cl-].[NH4+]>ClCCl>[Cl:8][C:9]1[N:14]=[C:13]([C:15]([N:6]([CH3:7])[CH3:5])=[O:16])[C:12]([C:18]([F:21])([F:20])[F:19])=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 674DimethylamineHCID 25517Ammonium ChlorideHCID 112990916-chloro-3-(trifluoromethyl)pyridine-2-carboxylic Acid

생성물 1

HCID 118020438HCID 118020438, 화합물수율 43%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

EDC (650 mg, 3.39 mmol) and dimethylamine (2.0 M solution in THF, 2.30 mL, 4.60 mmol) were added at room temperature to a solution of 6-chloro-3-(trifluoromethyl)pyridine-2-carboxylic acid (516 mg, 2.29 mmol) in dichloromethane (20 mL), and the mixture was stirred at room temperature for 4 hours. A saturated ammonium chloride aqueous solution was added to the reaction solution, followed by extraction with dichloromethane. The obtained organic layer was washed with brine and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography [elute: hexane/ethyl acetate=100/0-70/30 (gradient)] to obtain the title compound (246 mg, yield: 43%).

후처리

  1. extractionfollowed by extraction with dichloromethane
  2. washThe obtained organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography [elute: hexane/ethyl acetate=100/0-70/30 (gradient)]

출처 및 근거

ORD 기록
ord-c060cde2355f4a79b0555b9bd6f48ba0
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150575B2

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