Triethylamine → 1-(2,6-Diisopropyl-phenyl)-3-(5-tridecyl-[1,3,4]oxadiazol-2-yl)-urea

HRID 2081663ノート

反応式

HRID 2081663 の反応式
C(N(CC)CC)C.[NH2:8][C:9]1[O:10][C:11]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[N:12][N:13]=1.[CH:27]([C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([CH:36]([CH3:38])[CH3:37])[C:31]=1[N:39]=[C:40]=[O:41])([CH3:29])[CH3:28]>C(#N)C>[CH3:29][CH:27]([C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([CH:36]([CH3:37])[CH3:38])[C:31]=1[NH:39][C:40]([NH:8][C:9]1[O:10][C:11]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[N:12][N:13]=1)=[O:41])[CH3:28]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 922592,6-Diisopropylphenyl isocyanateHCID 105879212-Amino-5-tridecyl-1,3,4-oxadiazole

生成物 1

HCID 106480641-(2,6-Diisopropyl-phenyl)-3-(5-tridecyl-[1,3,4]oxadiazol-2-yl)-urea

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Triethylamine (1.67 g, 0.017 mol) was added to a solution of the compound prepared in Step 2 above (4.0 g, 0.015 mol) in acetonitrile (200 mL) and the mixture refluxed for 30 minutes or until solution becomes homogeneous. 2,6-Diisopropylphenyl isocyanate (3.71 g, 0.018 mol) was then added and reflux continued for 18 hours. The mixture was allowed to cool, concentrated, diluted with water (20 mL), filtered, and the solid columned on silica gel, eluting with 20% ethyl acetate in hexanes (loaded in chloroform) to give 0.54 g of a solid; m.p 114°-116.5° C.

後処理

  1. temperaturethe mixture refluxed for 30 minutes or until solution
  2. temperaturereflux
  3. temperatureto cool
  4. concentrationconcentrated
  5. additiondiluted with water (20 mL)
  6. filtrationfiltered
  7. washthe solid columned on silica gel, eluting with 20% ethyl acetate in hexanes (loaded in chloroform)

出典と根拠

ORDレコード
ord-1888fc7206f54f62a49636f9af4733d4
出典データセット
uspto-grants-1993_02
特許番号
US05185358

反応ノート

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