Sodium ethoxide → Chlorfenapyr

HRID 654134

反応式

HRID 654134 の反応式
[Br:1][C:2]1[C:3]([C:20]#[N:21])=[C:4]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=2)[N:5]([CH2:11]Cl)[C:6]=1[C:7]([F:10])([F:9])[F:8].[O-:22][CH2:23][CH3:24].[Na+]>C(O)C.O.CCOCC>[Br:1][C:2]1[C:3]([C:20]#[N:21])=[C:4]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=2)[N:5]([CH2:11][O:22][CH2:23][CH3:24])[C:6]=1[C:7]([F:10])([F:9])[F:8]

参加物

6

反応物 2

HCID 2723922Sodium ethoxideHCID 198886164-Bromo-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile

生成物 1

HCID 91778Chlorfenapyr収率 85.9%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

A solution of 4-bromo-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (2.0 g, 0.005 mol) in absolute ethanol is treated with a 21% wt/wt ethanolic solution of sodium ethoxide (0.36 g, 0.0053 mol), heated to 75°-80° C. for 20-30 minutes, cooled to room temperature and diluted with water and ether. The organic phase is dried over anhydrous magnesium sulfate and concentrated in vacuo to give a solid which is recrystallized form heptane to give the title product as a white solid (1.75 g, mp 97°-98° C.).

後処理

  1. temperatureheated to 75°-80° C. for 20-30 minutes
  2. dry with materialThe organic phase is dried over anhydrous magnesium sulfate
  3. concentrationconcentrated in vacuo
  4. customto give a solid which
  5. customis recrystallized form heptane

出典と根拠

ORDレコード
ord-d87701a3380848998d4943e36ed4b71b
出典データセット
uspto-grants-1992_07
特許番号
US05130328

関連ノート

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