1H-1,2,4-Triazole → HCID 68846595, 화합물

HRID 29225노트

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HRID 29225 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:21]=[C:22]([Cl:24])[CH:23]=1)[O:5][CH:6]([CH2:19][CH3:20])[C:7]([NH:9][C:10]([CH3:18])([CH3:17])[C:11]#[C:12][CH2:13][CH2:14][CH2:15]Cl)=[O:8].C(=O)([O-])[O-].[K+].[K+].[NH:31]1[CH:35]=[N:34][CH:33]=[N:32]1.CCCCCC.C(OCC)(=O)C>CN(C)C=O.O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:21]=[C:22]([Cl:24])[CH:23]=1)[O:5][CH:6]([CH2:19][CH3:20])[C:7]([NH:9][C:10]([CH3:18])([CH3:17])[C:11]#[C:12][CH2:13][CH2:14][CH2:15][N:31]1[CH:35]=[N:34][CH:33]=[N:32]1)=[O:8]

참가 물질

8

반응물 4

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 21226206Ethyl acetate hexaneHCID 68849646HCID 68849646, 화합물

생성물 1

HCID 68846595HCID 68846595, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
90 °C

실험 절차

To a stirred solution of 2-(3,5-dichlorophenoxy)-N-(1-chloro-6-methylhept-4-yn-6-yl) butyramide (0.59 g) in dry N,N-dimethylformamide (10 ml) containing anhydrous potassium carbonate (0.28 g) was added 1,2,4-triazole (0.10 g). The mixture was heated to 90° C. for 2.75 hours, cooled to ambient temperature, diluted with water and extracted with ethyl acetate (three times). The extracts were combined, washed with brine, dried over magnesium sulphate then evaporated under reduced pressure to give a yellow oil. The oil was fractionated by chromatography (silica; hexane/ethyl acetate, 2:1 by volume followed by ethyl acetate) to give the required product as a colourless oil, 0.16 g, 1H NMR (CDCl3) δ: 1.00-1.06(3H, t); 1.60(3H, s); 1.62(3H, s); 1.92-2.14(6H, m); 4.38-4.44(3H, m); 6.26(1H, s); 6.84(2H, s); 7.04(1H, s); 7.96(1H, s); 8.32(1H, s).

후처리

  1. temperaturecooled to ambient temperature
  2. extractionextracted with ethyl acetate (three times)
  3. washwashed with brine
  4. dry with materialdried over magnesium sulphate
  5. customthen evaporated under reduced pressure
  6. customto give a yellow oil

출처 및 근거

ORD 기록
ord-8f1f3b306b914e7fa27b6e94b11fb820
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07420090B2

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