1H-1,2,4-Triazole → HCID 68846595、化合物

HRID 29225ノート

反応式

HRID 29225 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 68846595HCID 68846595、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8f1f3b306b914e7fa27b6e94b11fb820
出典データセット
uspto-grants-2008_09
特許番号
US07420090B2

反応ノート

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