ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

p-Toluenesulfonic acid monohydrate → 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-5-formyl-N-(2-hydroxy-ethoxy)-benzamide

HRID 20722
ノート
印刷プレビュー

反応式

HRID 20722 の反応式
[Si]([O:8][CH2:9][CH2:10][O:11][NH:12][C:13](=[O:33])[C:14]1[CH:19]=[C:18]([CH:20]=[O:21])[C:17]([F:22])=[C:16]([F:23])[C:15]=1[NH:24][C:25]1[CH:30]=[CH:29][C:28]([I:31])=[CH:27][C:26]=1[F:32])(C(C)(C)C)(C)C.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>O1CCCC1.O>[F:23][C:16]1[C:15]([NH:24][C:25]2[CH:30]=[CH:29][C:28]([I:31])=[CH:27][C:26]=2[F:32])=[C:14]([CH:19]=[C:18]([CH:20]=[O:21])[C:17]=1[F:22])[C:13]([NH:12][O:11][CH2:10][CH2:9][OH:8])=[O:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 23132329N-[2-(t-butyldimethylsilanyloxy)-ethoxy]-3,4-difluoro-2-(2-fluoro-4-iodophenylamino)-5-formyl-benzamide

生成物 1

HCID 231323883,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-5-formyl-N-(2-hydroxy-ethoxy)-benzamide収率 72%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028
Tetrahydrofuran
溶媒

実験手順

N-[2-(Tert-butyldimethylsilanyloxy)-ethoxy]-3,4-difluoro-2-(2-fluoro-4-iodophenylamino)-5-formyl-benzamide (37.1 g as a crude product containing the desilylated product) prepared in Step E was dissolved in a mixed solvent of tetrahydrofuran (200 ml) and water (16 ml). To this solution, p-toluenesulfonic acid monohydrate (1.76 g, 9.25 mmol) was added, and the mixture was stirred at room temperature for 12 hours. The reaction mixture was extracted with ethyl acetate, and the organic layer was washed with saturated brine, dried over magnesium sulfate, and evaporated under reduced pressure. The resultant residue was triturated with ethyl acetate to give 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-5-formyl-N-(2-hydroxy-ethoxy)-benzamide (16.0 g, 72% yield in two steps) as a yellow solid.

後処理

  1. customprepared in Step E
  2. extractionThe reaction mixture was extracted with ethyl acetate
  3. washthe organic layer was washed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe resultant residue was triturated with ethyl acetate

出典と根拠

ORDレコード
ord-f60fcdef413646d4a7fb6a02472236dd
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745663B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート