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Imidazole → 4-(2-Imidazolylacetyl)benzenecarbonitrile

HRID 1825437
ノート
印刷プレビュー

反応式

HRID 1825437 の反応式
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]#[N:12])=[CH:7][CH:6]=1)=[O:4].[NH:13]1[CH:17]=[CH:16][N:15]=[CH:14]1>CC#N.ClCCl.O>[NH:13]1[CH:17]=[CH:16][N:15]=[C:14]1[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]#[N:12])=[CH:7][CH:6]=1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 795ImidazoleHCID 142493Benzonitrile, 4-(chloroacetyl)-

生成物 1

HCID 221429994-(2-Imidazolylacetyl)benzenecarbonitrile収率 90%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

A stirred solution of 4-(2-chloroacetyl)benzenecarbonitrile (0.5 M) and imidazole (1.5 M) in CH3CN (200 ml) were heated for 14 hours at 60° C. The product was stripped of solvent under reduced pressure. The residue was diluted with dichloromethane (250 ml) and water (100 ml), and the mixture was stirred for 30 min. After filtering off a solid impurity, the aqueous layer was removed and discarded. The organic layer was washed sequentially with water (60 ml), sat. aq. NaHCO3 (60 ml), water (60 ml), brine (60 ml), dried with Na2SO4, filtered, and concentrated under reduced pressure. The dark colored oil was dried overnight in vacuo giving 4-(2-imidazolylacetyl)benzenecarbonitrile in 90% yield.

後処理

  1. filtrationAfter filtering off a solid impurity
  2. customthe aqueous layer was removed
  3. washThe organic layer was washed sequentially with water (60 ml), sat. aq. NaHCO3 (60 ml), water (60 ml), brine (60 ml)
  4. dry with materialdried with Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe dark colored oil was dried overnight in vacuo

出典と根拠

ORDレコード
ord-64d88472578b4500b7925c35e9515b73
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07045519B2

反応ノート

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