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

HRID 2190128노트

반응식

HRID 2190128 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-75e573ea498546cdbafe8f6b5f8f2549
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08324268B2

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