Sodium Chloride → HCID 90017318, 화합물

HRID 1054997노트

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HRID 1054997 반응식
Cl[C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[C:4]([CH3:12])[N:3]=1.[CH3:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21][NH2:22])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].[Cl-].[Na+]>CN(C)C=O>[CH3:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21][NH:22][C:2]2[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[C:4]([CH3:12])[N:3]=2)=[CH:17][CH:16]=1

참가 물질

6

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HCID 5234Sodium ChlorideHCID 11430Potassium Carbonate2회HCID 754524-Methoxybenzylamine2회HCID 378634572-Chloro-6-methyl-3-(trifluoromethyl)pyridine

생성물 1

HCID 90017318HCID 90017318, 화합물수율 33.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

2-Chloro-6-methyl-3-(trifluoromethyl)pyridine (200 mg, 1.02 mmol, Eq: 1.00), (4-methoxyphenyl)methylamine (168 mg, 159 μL, 1.23 mmol, Eq: 1.2) and potassium carbonate (212 mg, 1.53 mmol, Eq: 1.5) were combined in dimethylformamide (1.2 mL) to give a light yellow suspension. The mixture was stirred at 120° C. for 2 h. Additional potassium carbonate (141 mg, 1.02 mmol, Eq: 1) and (4-methoxyphenyl)methanamine (140 mg, 133 μL, 1.02 mmol, Eq: 1) were added and the mixture was stirred at 120° C. for 7 h. Saturated aqueous sodium chloride solution was added and the mixture was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated to an oil. The product (100 mg, 33%) was obtained as a colorless oil by column chromatography (SiO2, ethyl acetate/n-heptane). MS: m/z=297.3 (M+H+)

후처리

  1. customto give a light yellow suspension
  2. stirringthe mixture was stirred at 120° C. for 7 h
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. concentrationconcentrated to an oil

출처 및 근거

ORD 기록
ord-14648523ceed49cdb7ba63ee5c513b60
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394311B2

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