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

HRID 1036992ノート

反応式

HRID 1036992 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b19f6e7d2d65412492d0693e23f889c6
出典データセット
uspto-grants-2013_10
特許番号
US08546438B2

反応ノート

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