Water → HCID 14054586, 화합물

HRID 1381986노트

반응식

HRID 1381986 반응식
[NH2:1][CH:2]([CH:5]([CH3:7])[CH3:6])[C:3]#[N:4].C(N(CC)CC)C.[Cl:15][C:16]1[CH:17]=[C:18]([CH:22]=[CH:23][N:24]=1)[C:19](Cl)=[O:20].O>C(Cl)Cl.C(OCC)(=O)C>[C:3]([CH:2]([NH:1][C:19](=[O:20])[C:18]1[CH:22]=[CH:23][N:24]=[C:16]([Cl:15])[CH:17]=1)[CH:5]([CH3:7])[CH3:6])#[N:4]

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 28000032-Chloropyridine-4-carbonyl chlorideHCID 104191372-Amino-3-methylbutyronitrile

생성물 1

HCID 14054586HCID 14054586, 화합물수율 84.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

2.0 g (0.02 mol) of 2-amino-3-methylbutyronitrile and 2.8 ml (0.02 mol) of triethylamine were dissolved in 30 ml of methylene chloride. The solution was cooled to 10° C. or below and 3.0 g (0.017 mol) of 2-chloroisonicotinoyl chloride was added dropwise thereto at 10° C. or below lest unfavorable heat generation should occur. Then, the mixture was stirred at room temperature for 1.5 h to conduct a reaction. Water and ethyl acetate were added thereto to conduct extraction. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated to obtain an oil, which was purified according to silica gel column chromatography to obtain 3.4 g (yield: 84.1%) of the intended product in the form of a colorless oil.

후처리

  1. temperatureThe solution was cooled to 10° C. or below
  2. customat 10° C. or below
  3. customa reaction
  4. extractionextraction
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. customto obtain an oil, which
  9. customwas purified

출처 및 근거

ORD 기록
ord-28ed7540e052408fb994dbfb08c66436
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804762

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