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Sodium Iodide → N-(1-{2-[3-(2,6-Dimethyl-pyridin-4-yl)-ureido]-ethyl}-piperidin-4-yl)-N-ethyl-4-methoxy-benzenesulfonamide

HRID 2354076
ノート
印刷プレビュー

反応式

HRID 2354076 の反応式
[CH2:1]([N:3]([CH:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)[S:4]([C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=1)(=[O:6])=[O:5])[CH3:2].C([O-])(O)=O.[Na+].[Na+].[I-].Cl[CH2:29][CH2:30][NH:31][C:32]([NH:34][C:35]1[CH:40]=[C:39]([CH3:41])[N:38]=[C:37]([CH3:42])[CH:36]=1)=[O:33]>C1COCC1>[CH3:41][C:39]1[CH:40]=[C:35]([NH:34][C:32](=[O:33])[NH:31][CH2:30][CH2:29][N:18]2[CH2:19][CH2:20][CH:15]([N:3]([CH2:1][CH3:2])[S:4]([C:7]3[CH:8]=[CH:9][C:10]([O:13][CH3:14])=[CH:11][CH:12]=3)(=[O:5])=[O:6])[CH2:16][CH2:17]2)[CH:36]=[C:37]([CH3:42])[N:38]=1
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

6

反応物 4

HCID 5238Sodium IodideHCID 516892Sodium BicarbonateHCID 588165671-(2-Chloro-ethyl)-3-(2,6-dimethyl-pyridin-4-yl)-ureaHCID 58816568N-Ethyl-4-methoxy-N-piperidin-4-yl-benzenesulfonamide

生成物 1

HCID 11294764N-(1-{2-[3-(2,6-Dimethyl-pyridin-4-yl)-ureido]-ethyl}-piperidin-4-yl)-N-ethyl-4-methoxy-benzenesulfonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

A suspension of N-ethyl-4-methoxy-N-piperidin-4-yl-benzenesulfonamide (Example A4., 2.09 g, 7.0 mmol), NaHCO3 (3.4 g, 40 mmol), NaI (0.75 g, 5 mmol) and 1-(2-chloro-ethyl)-3-(2,6-dimethyl-pyridin-4-yl)-urea (Example D1, 1.14 g 5 mmol) in THF (30 mL) is stirred at 50° C. for 27 days. The mixture is quenched with Na2CO3 (150 mL) and extracted with CH2Cl2 (3×100 mL). The organic extracts are washed with sat. aq. Na2CO3 (70 mL), dried (Na2SO4), filtered and evaporated. The residue is purified by MPLC to provide the title compound.

後処理

  1. customThe mixture is quenched with Na2CO3 (150 mL)
  2. extractionextracted with CH2Cl2 (3×100 mL)
  3. washThe organic extracts are washed with sat. aq. Na2CO3 (70 mL)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by MPLC

出典と根拠

ORDレコード
ord-1b4808b58ec74821946649715966a947
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07750161B2

反応ノート

読み込み中…

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