Hydrochloric Acid → 5-(3-Chloro-5-fluorophenyl)-4-(3-cyanophenyl)thiophene-2-carboxylic acid

HRID 1036992노트

반응식

HRID 1036992 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2[S:13][C:12]([C:14]([O:16]CC)=[O:15])=[CH:11][C:10]=2[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([C:25]#[N:26])[CH:20]=2)[CH:5]=[C:6]([F:8])[CH:7]=1.[OH-].[Li+].O.Cl>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2[S:13][C:12]([C:14]([OH:16])=[O:15])=[CH:11][C:10]=2[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([C:25]#[N:26])[CH:20]=2)[CH:5]=[C:6]([F:8])[CH:7]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 58066751Ethyl 5-(3-chloro-5-fluorophenyl)-4-(3-cyanophenyl)thiophene-2-carboxylate

생성물 1

HCID 580667575-(3-Chloro-5-fluorophenyl)-4-(3-cyanophenyl)thiophene-2-carboxylic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

130 mg (0.34 mmol) of the compound from Example 11A are provided in 6.1 ml of tetrahydrofuran, and 80.7 mg (3.37 mmol) of lithium hydroxide and 2.0 ml of water are added at room temperature. The mixture is stirred at room temperature overnight, a 1N aqueous HCl solution is subsequently added until an acidic pH is obtained, the mixture is extracted with ethyl acetate and the extract is dried over sodium sulfate, filtered and concentrated. 119 mg (89% of theory) of the title compound are obtained.

후처리

  1. customis obtained
  2. extractionthe mixture is extracted with ethyl acetate
  3. dry with materialthe extract is dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b19f6e7d2d65412492d0693e23f889c6
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546438B2

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