苦味酸 → 1-Allyl-alpha-(p-chlorophenyl)-alpha-phenylimidazole-2-methanol

HRID 261964

反应方程式

HRID 261964 反应方程式
[CH2:1](Br)[CH:2]=[CH2:3].[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([C:14]2[NH:15][CH:16]=[CH:17][N:18]=2)[OH:13])=[CH:8][CH:7]=1.[OH-].[Na+].C1(C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C=1)[N+]([O-])=O>C(#N)C>[CH2:1]([N:15]1[CH:16]=[CH:17][N:18]=[C:14]1[C:12]([C:9]1[CH:8]=[CH:7][C:6]([Cl:5])=[CH:11][CH:10]=1)([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[OH:13])[CH:2]=[CH2:3]

参与物

6

反应物 4

HCID 6954苦味酸HCID 78413-溴丙烯HCID 14798二甲基对苯二胺二盐酸HCID 12433863(4-chlorophenyl)(1H-imidazol-2-yl)phenylmethanol

产物 1

HCID 124339291-Allyl-alpha-(p-chlorophenyl)-alpha-phenylimidazole-2-methanol

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

A mixture of 3.4 g (0.028 mol) of freshly distilled allyl bromide, 7 g (0.025 mol) of α-(p-chlorophenyl)-α-phenylimidazole-2-methanol (prepared according to Example IV), 1.2 g (0.030 mol) of sodium hydroxide, 0.050 g of picric acid and 50 ml. of acetonitrile was refluxed for 5 hours. The warm reaction mixture was filtered and water was added to the filtrate. The precipitate formed was filtered off, washed with water and petroleum ether (boiling range 40°-60° C.) and three times crystallised from isopropyl alcohol. 1-Allyl-α-(p-chlorophenyl)-α-phenylimidazole-2-methanol was obtained. Melting point 165°-165.5° C.

后处理

  1. customThe warm reaction mixture
  2. filtrationwas filtered
  3. additionwater was added to the filtrate
  4. customThe precipitate formed
  5. filtrationwas filtered off
  6. washwashed with water and petroleum ether (boiling range 40°-60° C.) and three times
  7. customcrystallised from isopropyl alcohol

来源与证据

ORD记录
ord-9019765763da459a8ba96ec7d4673355
来源数据集
uspto-grants-1979_05
专利号
US04152441

关联笔记

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