三乙胺 → 1-(2,6-Diisopropyl-phenyl)-3-(5-tridecyl-[1,3,4]oxadiazol-2-yl)-urea

HRID 2081663笔记

反应方程式

HRID 2081663 反应方程式
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]

参与物

5

反应物 3

HCID 8471三乙胺HCID 922592,6-二异丙基苯异氰酸酯HCID 105879212-Amino-5-tridecyl-1,3,4-oxadiazole

产物 1

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

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

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.

后处理

  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)

来源与证据

ORD记录
ord-1888fc7206f54f62a49636f9af4733d4
来源数据集
uspto-grants-1993_02
专利号
US05185358

反应笔记

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