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Hydrochloric Acid → N-[3-Carbamoyl-4-[1-(4,5-dihydro-3H-pyrrol-2-yl)piperidin-4-yloxy]phenyl]-N-[3-[3-(ethoxycarbonylamino)(imino)methylphenyl]-2-(E)-propeny]methanesulfonamide Dihydrochloride

HRID 1796192
ノート
印刷プレビュー

反応式

HRID 1796192 の反応式
[ClH:1].Cl.C([C:6]1[CH:7]=[C:8](/[CH:12]=[CH:13]/[CH2:14][N:15]([C:20]2[CH:25]=[CH:24][C:23]([O:26][CH:27]3[CH2:32][CH2:31][N:30]([C:33]4[CH2:37][CH2:36][CH2:35][N:34]=4)[CH2:29][CH2:28]3)=[C:22]([C:38](=[O:40])[NH2:39])[CH:21]=2)[S:16]([CH3:19])(=[O:18])=[O:17])[CH:9]=[CH:10][CH:11]=1)(=N)N.[C:41](=[O:55])([O:45][C:46]1[CH:51]=CC([N+]([O-])=O)=CC=1)OCC.C([N:58]([CH2:61]C)CC)C.Cl.C[N:65](C)C=O>ClCCl.O1CCOCC1.O>[ClH:1].[ClH:1].[C:38]([C:22]1[CH:21]=[C:20]([N:15]([CH2:14]/[CH:13]=[CH:12]/[C:8]2[CH:9]=[CH:10][CH:11]=[C:6]([NH:65][C:41]([O:45][CH2:46][CH3:51])=[O:55])[C:7]=2[CH:61]=[NH:58])[S:16]([CH3:19])(=[O:18])=[O:17])[CH:25]=[CH:24][C:23]=1[O:26][CH:27]1[CH2:32][CH2:31][N:30]([C:33]2[CH2:37][CH2:36][CH2:35][N:34]=2)[CH2:29][CH2:28]1)(=[O:40])[NH2:39]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 8471TriethylamineHCID 586863Ethyl 4-nitrophenyl carbonateHCID 22180975N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[3-carbamoyl-4-[1-(4,5-dihydro-3H-pyrrol-2-yl)piperidin-4-yloxy]phenyl]methanesulfonamide dihydrochloride

生成物 1

HCID 86593745
N-[3-Carbamoyl-4-[1-(4,5-dihydro-3H-pyrrol-2-yl)piperidin-4-yloxy]phenyl]-N-[3-[3-(ethoxycarbonylamino)(imino)methylphenyl]-2-(E)-propeny]methanesulfonamide Dihydrochloride
収率 84%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回HCID 312751,4-Dioxane溶媒

実験手順

To a solution of N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[3-carbamoyl-4-[1-(4,5-dihydro-3H-pyrrol-2-yl)piperidin-4-yloxy]phenyl]methanesulfonamide dihydrochloride (0.23 g) obtained in example 99(b) in a mixture of dichloromethane (4.5 ml) and N,N-dimethylformamide (1.5 ml) were added successively ethyl 4-nitrophenyl carbonate (0.10 g) obtained in example 103 and triethylamine (0.16 ml) at room temperature, and the resulting mixture was stirred at room temperature overnight and then evaporated in vacuo. The residue obtained was purified by chromatography on a silica gel column using a mixed solvent of dichloromethane and methanol (50:0˜47:3). Subsequently, to a solution of the oily product obtained in ethanol (2 ml) was added a 4N solution of hydrogen chloride in dioxane (0.5 ml), and the resulting mixture was evaporated to dryness in vacuo. The amorphous solid obtained was dissolved in dichloromethane, and the resulting mixture was extracted with 1N hydrochloric acid, and the aqueous layer collected was evaporated in vacuo. The residue obtained was dissolved in water and then lyophilized to afford the title compound (0.20 g, yield: 84%) as a colorless amorphous solid.

後処理

  1. customevaporated in vacuo
  2. customThe residue obtained
  3. customwas purified by chromatography on a silica gel column
  4. customSubsequently, to a solution of the oily product obtained in ethanol (2 ml)
  5. customthe resulting mixture was evaporated to dryness in vacuo
  6. customThe amorphous solid obtained
  7. extractionthe resulting mixture was extracted with 1N hydrochloric acid
  8. customthe aqueous layer collected
  9. customwas evaporated in vacuo
  10. customThe residue obtained

出典と根拠

ORDレコード
ord-de93b66ab61d41a6949b572767a08711
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07030138B2

反応ノート

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