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Sodium Hydroxide → 3-(2-Fluoro-4-methylsulfanyl-phenylamino)-thieno[3,2-c]pyridine-2-carboxylic acid

HRID 1366796
ノート
印刷プレビュー

反応式

HRID 1366796 の反応式
C([O:3][C:4]([C:6]1[S:14][C:13]2[CH:12]=[CH:11][N:10]=[CH:9][C:8]=2[C:7]=1[NH:15][C:16]1[CH:21]=[CH:20][C:19]([S:22][CH3:23])=[CH:18][C:17]=1[F:24])=[O:5])C.[OH-].[Na+]>>[F:24][C:17]1[CH:18]=[C:19]([S:22][CH3:23])[CH:20]=[CH:21][C:16]=1[NH:15][C:7]1[C:8]2[CH:9]=[N:10][CH:11]=[CH:12][C:13]=2[S:14][C:6]=1[C:4]([OH:5])=[O:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 597038903-(2-Fluoro-4-methylsulfanyl-phenylamino)-thieno[3,2-c]pyridine-2-carboxylic acid ethyl ester

生成物 1

HCID 597039013-(2-Fluoro-4-methylsulfanyl-phenylamino)-thieno[3,2-c]pyridine-2-carboxylic acid収率 61.5%

反応条件

温度
60 °C

実験手順

A suspension of 3-(2-fluoro-4-methylsulfanyl-phenylamino)-thieno[3,2-c]pyridine-2-carboxylic acid ethyl ester (0.19 g, 0.52 mmol) in IMS (10 ml) was treated with sodium hydroxide (1M aqueous solution, 0.63 ml) and the reaction mixture heated at 60° C. for 3 hours. The resultant mixture was allowed to cool then concentrated in vacuo. The crude residue was treated with water and the mixture adjusted to pH 5 with acetic acid. The resultant suspension was filtered, the residue collected and dried in vacuo to give the title compound as a green solid (0.107 g, 56%) which was used without purification in the subsequent step.

後処理

  1. temperatureto cool
  2. concentrationthen concentrated in vacuo
  3. additionThe crude residue was treated with water
  4. filtrationThe resultant suspension was filtered
  5. customthe residue collected
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-c2664d17976643b6b3f0f9bfe6d0cd39
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07893085B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート