反応 #792140

ord-d141f4d160b54c5593da59aedd2a5554

反応方程式

[Na+].[OH-]
sodium hydroxide
c1c[nH]nn1
triazole
CCC1(c2ccc(Oc3ccc(Cl)cc3)cc2Cl)CO1
2-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-ethyl-oxirane
CN1CCCC1=O
N-methyl-2-pyrrolidon
[Cl-].[NH4+]
ammonium chloride
CCC(O)(Cn1cncn1)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)butan-2-ol

反応条件

温度
140°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the mixture extracted with MTBE
  2. 2
    洗浄washed with an aqueous solution of lithium chloride
  3. 3
    その他The crude residue was purified by recrystallization in diisopropylether

実験手順

To 2-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-ethyl-oxirane (216.0 g, 0.63 mol) dissolved in N-methyl-2-pyrrolidon (2 L) was added sodium hydroxide (62.87 g, 1.57 mol) and triazole (217.1 g, 3.14 mol) at room temperature. The mixture was then stirred for 12 hours at 140° C. A solution of ammonium chloride and ice water was then added, the mixture extracted with MTBE and washed with an aqueous solution of lithium chloride. The crude residue was purified by recrystallization in diisopropylether to give 2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)butan-2-ol compound as a colorless solid (127.0 g, 51%; m.p.=140-142° C.).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09173402B2uspto-grants-2015_11