Benzyl Chloride → 4-(dibenzylamino)furan-2(5H)-one

HRID 451341ノート

反応式

HRID 451341 の反応式
[CH2:1]([NH:8][C:9]1[CH2:13][O:12][C:11](=[O:14])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].[CH2:17](Cl)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(COC)OC>[CH2:1]([N:8]([CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:9]1[CH2:13][O:12][C:11](=[O:14])[CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 7503Benzyl ChlorideHCID 14798Sodium HydroxideHCID 134024534-(benzylamino)furan-2(5H)-one

生成物 1

HCID 684873224-(dibenzylamino)furan-2(5H)-one収率 68%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
50 °C

実験手順

6.3 g of 4-(benzylamino)furan-2(5H)-one (Example 16) are initially charged in 75 ml of dimethoxyethane at room temperature. Subsequently, 1.1 g of sodium hydroxide are added and, at 40° C., 4 g of benzyl chloride are metered in. The mixture is stirred at 50° C. for a further 7 h. The solvent is substantially removed under reduced pressure and the residue is admixed with 50 ml of water and 50 ml of methylene chloride. The organic phase is removed, and the aqueous phase is extracted once again with 50 ml of methylene chloride. The combined methylene chloride phases are dried over sodium sulphate and the solvent is removed under reduced pressure. 5.6 g of 4-(dibenzylamino)furan-2(5H)-one are obtained (this corresponds to 68% yield).

後処理

  1. customThe solvent is substantially removed under reduced pressure
  2. customThe organic phase is removed
  3. extractionthe aqueous phase is extracted once again with 50 ml of methylene chloride
  4. dry with materialThe combined methylene chloride phases are dried over sodium sulphate
  5. customthe solvent is removed under reduced pressure

出典と根拠

ORDレコード
ord-99d4422681b74dcaa7c70815eb5e977e
出典データセット
uspto-grants-2013_07
特許番号
US08487112B2

反応ノート

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