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Glutaraldehyde → HCID 178522094、化合物

HRID 491796
ノート
印刷プレビュー

反応式

HRID 491796 の反応式
Cl.Cl.[NH2:3][C@H:4]1[CH2:9][CH2:8][C@H:7]([C:10]([NH:12][C:13]2[C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=3[O:15][C:14]=2[C:22]([NH:24][C:25]2[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][N:26]=2)=[O:23])=[O:11])[CH2:6][CH2:5]1.[CH:32](=O)[CH2:33][CH2:34][CH2:35][CH:36]=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>ClCCl.C(N(CC)CC)C>[N:3]1([C@H:4]2[CH2:9][CH2:8][C@H:7]([C:10]([NH:12][C:13]3[C:17]4[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=4[O:15][C:14]=3[C:22]([NH:24][C:25]3[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][N:26]=3)=[O:23])=[O:11])[CH2:6][CH2:5]2)[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 3485GlutaraldehydeHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 178478721HCID 178478721、化合物

生成物 1

HCID 178522094HCID 178522094、化合物収率 85.6%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane
溶媒
HCID 8471Triethylamine溶媒

実験手順

Trans-3-(4-aminocyclohexylcarbonylamino)-N-(5-chloropyridin-2-yl)benzofuran-2-carboxamide dihydrochloride (125 mg) obtained in Example 219 is suspended in dichloromethane (10 ml), and thereto is added triethylamine (102 μl) under ice-cooling, and the mixture is stirred for several minutes. Then, about 25% aqueous glutaraldehyde solution (150 mg) and sodium triacetoxy borohydride (155 mg) are added successively, and the mixture is stirred under ice-cooling for 2 hours. To the reaction solution is poured a saturated aqueous sodium hydrogen carbonate solution, and the mixture is extracted with chloroform. The organic layer is washed successively with water and a saturated brine, dried over sodium sulfate, and the solvent is evaporated under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (eluent: n-hexane/ethyl acetate=3/1, then 1/1) to give trans-3-[4-(piperidin-1-yl)cyclohexylcarbonylamino]-N-(5-chloropyridin-2-yl)benzofuran-2-carboxamide (106 mg). Subsequently, this product is dissolved in chloroform/methanol (5/1, 6 ml), and 4N hydrogen chloride in ethyl acetate (5 ml) is added thereto under ice-cooling. The reaction solution is concentrated under reduced pressure, and the resulting residue is suspended in diethyl ether, and collected by filtration to give the title compound (107 mg).

後処理

  1. temperaturecooling
  2. stirringthe mixture is stirred under ice-
  3. temperaturecooling for 2 hours
  4. extractionthe mixture is extracted with chloroform
  5. washThe organic layer is washed successively with water
  6. dry with materiala saturated brine, dried over sodium sulfate
  7. customthe solvent is evaporated under reduced pressure
  8. customThe resulting residue is purified by NH-silica gel column chromatography (eluent

出典と根拠

ORDレコード
ord-ef9f451ec58b4192b62dedfb623a4482
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531537B2

反応ノート

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