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

Diethylamine → 3-[3-(2-diethylamino-ethyl)-3H-isobenzofuran-1-ylidene]-1,3-dihydro-indol-2-one

HRID 1829054
ノート
印刷プレビュー

反応式

HRID 1829054 の反応式
[O:1]=[C:2]1[C:10](=[C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:13]([CH2:20][CH2:21]OS(C)(=O)=O)[O:12]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[NH:3]1.[CH2:27]([NH:29][CH2:30][CH3:31])[CH3:28].O1CCOCC1>C1COCC1>[CH2:27]([N:29]([CH2:30][CH3:31])[CH2:21][CH2:20][CH:13]1[C:14]2[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:11](=[C:10]2[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[NH:3][C:2]2=[O:1])[O:12]1)[CH3:28]
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 3

HCID 8021DiethylamineHCID 312751,4-DioxaneHCID 72382355Methanesulfonic Acid 2-[3-(2-oxo-1,2-dihydro-indol-3-ylidene)-1,3-dihydro-isobenzofuran-1-yl]-ethyl Ester

生成物 1

HCID 696592283-[3-(2-diethylamino-ethyl)-3H-isobenzofuran-1-ylidene]-1,3-dihydro-indol-2-one収率 71%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of methanesulfonic acid 2-[3-(2-oxo-1,2-dihydro-indol-3-ylidene)-1,3-dihydro-isobenzofuran-1-yl]-ethyl ester (50 mg, 0.135 mmol) and diethylamine (279 μl, 2.7 mmol) in THF (0.8 ml) was heated at 60° C. After 3 hours, dioxane (0.3 ml) was added to give a solution and the reaction continued at 60° C. for 24 h. The reaction was partitioned between EtOAc and water. The EtOAc layer was washed with water, brine, dried with anhydrous Na2SO4 and rotary evaporated to give brown oil. The brown oil was chromatographed (CHCl3 to 2% MeOH/CHCl3 gradient) to yield 3-[3-(2-diethylamino-ethyl)-3H-isobenzofuran-1-ylidene]-1,3-dihydro-indol-2-one as a yellow-green solid (33 mg, 71%).

後処理

  1. customto give a solution
  2. waitthe reaction continued at 60° C. for 24 h
  3. customThe reaction was partitioned between EtOAc and water
  4. washThe EtOAc layer was washed with water, brine
  5. dry with materialdried with anhydrous Na2SO4
  6. customrotary evaporated
  7. customto give brown oil
  8. customThe brown oil was chromatographed (CHCl3 to 2% MeOH/CHCl3 gradient)

出典と根拠

ORDレコード
ord-b82f502a9b71451797c94ced6f5ca5f7
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07060844B2

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