Lithium Hydroxide → 4,5-Bis(3-chlorophenyl)furan-2-carboxylic acid

HRID 2190128ノート

反応式

HRID 2190128 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[C:10]([C:20]([O:22]CC)=[O:21])[O:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)[CH:5]=[CH:6][CH:7]=1.[OH-].[Li+]>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[C:10]([C:20]([OH:22])=[O:21])[O:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 58064774Ethyl 4,5-bis(3-chlorophenyl)furan-2-carboxylate

生成物 1

HCID 580647634,5-Bis(3-chlorophenyl)furan-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
50 °C

実験手順

760 mg (2.10 mmol) of the compound from Example 14A are provided in 20 ml of dioxane, and 20 ml of a 2N aqueous lithium hydroxide solution are added at room temperature. The mixture is stirred at 50° C. for two hours and subsequently concentrated. A 1N aqueous HCl solution is then added until an acidic pH is established, the mixture is extracted with dichloromethane and the organic phase is dried over magnesium sulfate, filtered and concentrated. 401 mg (57% of theory) of the title compound are obtained.

後処理

  1. concentrationsubsequently concentrated
  2. additionA 1N aqueous HCl solution is then added until an acidic pH
  3. extractionthe mixture is extracted with dichloromethane
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-75e573ea498546cdbafe8f6b5f8f2549
出典データセット
uspto-grants-2012_12
特許番号
US08324268B2

反応ノート

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