Lithium Hydroxide → 3-Bromo-4-(4-trifluoromethyl-benzyl)-4H-thieno[3,2-b]pyrrole-5-carboxylic acid

HRID 1951644ノート

反応式

HRID 1951644 の反応式
C[O:2][C:3]([C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=2)[C:8]2[C:21]([Br:24])=[CH:22][S:23][C:7]=2[CH:6]=1)=[O:4].[Li+].[OH-]>CO.C1COCC1>[Br:24][C:21]1[C:8]2[N:9]([CH2:10][C:11]3[CH:16]=[CH:15][C:14]([C:17]([F:18])([F:20])[F:19])=[CH:13][CH:12]=3)[C:5]([C:3]([OH:4])=[O:2])=[CH:6][C:7]=2[S:23][CH:22]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 582976733-Bromo-4-(4-trifluoromethyl-benzyl)-4H-thieno[3,2-b]pyrrole-5-carboxylic acid methyl ester

生成物 1

HCID 582976983-Bromo-4-(4-trifluoromethyl-benzyl)-4H-thieno[3,2-b]pyrrole-5-carboxylic acid

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

反応条件

温度
55 °C

実験手順

To a solution of the crude product of Step 3 (4 g) in 50 ml of 1:1 MeOH/THF was added 25 ml of 1N aqueous LiOH solution. The reaction mixture was stirred at 55° C. for 4 h and the concentrated under reduced pressure to move the volatile solvent. The resulting aqueous solution was treated with 5 ml of AcOH and stirred for 2 h. The solid was collected by filtration to give 3.2 of the title compound as a white powder.

後処理

  1. concentrationthe concentrated under reduced pressure
  2. additionThe resulting aqueous solution was treated with 5 ml of AcOH
  3. stirringstirred for 2 h
  4. filtrationThe solid was collected by filtration

出典と根拠

ORDレコード
ord-38c4d35a2e3347259536df4abfb41df9
出典データセット
uspto-grants-2013_03
特許番号
US08404736B2

反応ノート

読み込み中…