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Dimethylamine → 1-(6-Chloropyridin-3-yl)-N,N-dimethylmethanamine

HRID 1455077
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HRID 1455077 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]Cl)=[CH:4][N:3]=1.[CH3:10][NH:11][CH3:12].C(=O)([O-])[O-].[K+].[K+].O>C(O)C>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([CH2:8][N:11]([CH3:12])[CH3:10])=[CH:6][CH:7]=1
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참가 물질

6

반응물 4

HCID 674DimethylamineHCID 962WaterHCID 11430Potassium CarbonateHCID 1554792-Chloro-5-(chloromethyl)pyridine

생성물 1

HCID 120566771-(6-Chloropyridin-3-yl)-N,N-dimethylmethanamine

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

2-Chloro-5-(chloromethyl)pyridine (500 mg) was dissolved in ethanol (7.0 ml). dimethylamine (0.83 ml, 33% in ethanol) and potassium carbonate (641 mg) were added and the resulting mixture was refluxed for 1.5 hours. After evaboration of ethanol, water was added and the aqueous mixture was extracted with ethyl acetate. 1H NMR (400 MHz, d6-DMSO) δ: 8.31 (d, 1H, J 2.3 Hz), 7.77 (dd, 1H, J 8.2, 2.3 Hz), 7.47 (d, 1H, J 8.2 Hz), 3.41 (s, 2H), 2.14 (s, 6H).

후처리

  1. temperaturethe resulting mixture was refluxed for 1.5 hours
  2. extractionthe aqueous mixture was extracted with ethyl acetate

출처 및 근거

ORD 기록
ord-a72f5db53d9240e08e12fcd5aba29a27
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07482340B2

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