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Triethylamine → HCID 44574294, 화합물

HRID 1878062
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HRID 1878062 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[N:9])=[CH:4][N:3]=1.C(N(CC)CC)C.[Cl:17][CH:18]([CH3:22])[C:19](Cl)=[O:20]>ClCCl>[Cl:17][CH:18]([CH3:22])[C:19]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[N:9])=[CH:4][N:3]=1)=[O:20]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 1110192-Chloropropionyl chlorideHCID 8182602-Amino-5-cyanopyridine

생성물 1

HCID 44574294HCID 44574294, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

To a suspension of 2-amino-5-cyanopyridine (0.500 g, 4.2 mmol) in dry dichloromethane (20 mL) was added triethylamine (0.830 g, 6.3 mmol) and the mixture was stirred at 0° C. To the reaction mixture, 2-chloropropionyl chloride (0.800 g, 6.3 mmol) was added dropwise, and the reaction mixture was stirred at 0° C. for an hour and then at room temperature for 48 hours. The reaction mixture was diluted with dichloromethane (100 mL) and was washed with water (150 mL). The reaction mixture was dried over anhydrous sodium sulfate and concentrated to obtain the crude product, which was purified by column chromatography (silica gel, 15-20% ethyl acetate in petroleum ether as an eluent) to obtain the title compound.

후처리

  1. stirringthe reaction mixture was stirred at 0° C. for an hour
  2. washwas washed with water (150 mL)
  3. dry with materialThe reaction mixture was dried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customto obtain the crude product, which
  6. customwas purified by column chromatography (silica gel, 15-20% ethyl acetate in petroleum ether as an eluent)

출처 및 근거

ORD 기록
ord-2cc7b6b7adcc41ceaa2c0a1f37fa61f1
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08314103B2

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