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Piperidin-4-ol → 1-(4-(4-Bromophenylsulfonyl)phenyl)-3-(3-((4-hydroxypiperidin-1-yl)(imino)methyl)phenyl)urea

HRID 1797935
ノート
印刷プレビュー

反応式

HRID 1797935 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH:17][C:18]([NH:20][C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([C:27]#[N:28])[CH:22]=3)=[O:19])=[CH:13][CH:12]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(C1C=C(NC(=O)N)C=CC=1)#N.[NH:41]1[CH2:46][CH2:45][CH:44]([OH:47])[CH2:43][CH2:42]1>Cl.O1CCOCC1.CO>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([C:11]2[CH:12]=[CH:13][C:14]([NH:17][C:18]([NH:20][C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([C:27]([N:41]4[CH2:46][CH2:45][CH:44]([OH:47])[CH2:43][CH2:42]4)=[NH:28])[CH:22]=3)=[O:19])=[CH:15][CH:16]=2)(=[O:10])=[O:9])=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 79341Piperidin-4-olHCID 206364711-(3-Cyanophenyl)ureaHCID 57504036HCID 57504036、化合物

生成物 1

HCID 575040281-(4-(4-Bromophenylsulfonyl)phenyl)-3-(3-((4-hydroxypiperidin-1-yl)(imino)methyl)phenyl)urea

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒
HCID 21966525
Dioxane Methanol
溶媒

実験手順

Under argon atmosphere, 1 equivalent of 1-(4-(4-bromophenylsulfonyl)phenyl)-3-(3-cyanophenyl)urea (VIII) [or a correspondent 14444-substituted-phenylsulfonyl)phenyl)-3-(3-cyanophenyl)urea] was dissolved in of 4 M HCl in dioxane/MeOH 5:1. The solution was stirred overnight at rt then the solvent was removed in vacuo. The residue was washed with diethylether, dried in vacuo, dissolved in dry MeOH (or DMF) and reacted with 1.1 to 2 equivalents of piperidin-4-ol (or 1.1 to 2 equivalents of the corresponding secondary amine) at temperature between 55 and 70° C. for a minimum of 4 h to a maximum of 22 h. The products were purified either by flash chromatography, using a silica gel column and an appropriate gradient of MeOH in DCM as eluent, or by preparative HPLC, using a reverse-phase column and a gradient of acetonitrile in 0.1% HCOOHaq.

後処理

  1. customthe solvent was removed in vacuo
  2. washThe residue was washed with diethylether
  3. customdried in vacuo
  4. dissolutiondissolved in dry MeOH (or DMF)
  5. customThe products were purified either by flash chromatography

出典と根拠

ORDレコード
ord-26a1059800b6428da30c7c35f22aad99
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08343963B2

反応ノート

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