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乙醇 → HCID 23627582,化合物

HRID 1663262
笔记
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反应方程式

HRID 1663262 反应方程式
C(C1C=CC(CC[CH:11]([CH:15]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[C:22]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[N:16]2[S:29]([C:32]2[CH:37]=[CH:36][C:35]([Cl:38])=[C:34]([Cl:39])[CH:33]=2)(=[O:31])=[O:30])[C:12]([NH2:14])=[O:13])=CC=1)#N.C(=O)([O-])[O-].[NH4+:44].[NH4+:45].[CH2:46](O)[CH3:47]>Cl>[C:23]([C:22]1[CH:21]=[CH:20][C:19]([CH2:46][CH2:47][NH:14][C:12](=[O:13])[CH2:11][CH:15]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[C:22]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[N:16]2[S:29]([C:32]2[CH:37]=[CH:36][C:35]([Cl:38])=[C:34]([Cl:39])[CH:33]=2)(=[O:30])=[O:31])=[CH:18][CH:17]=1)(=[NH:45])[NH2:44]
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 702乙醇HCID 517111碳酸铵HCID 86635301HCID 86635301,化合物

产物 1

HCID 23627582HCID 23627582,化合物收率 55%

试剂、催化剂与溶剂 1

HCID 313盐酸溶剂

实验过程

A solution of N-[2-(4-cyano-phenyl)-ethyl]-2-[5-(3,4-dichloro-benzenesulfonyl)-5,6-dihydro-phenanthridin-6-yl]-acetamide (Example 7) (200 mg, 0.35 mmol) in 9M hydrogen chloride in ethanol (10 mL) was allowed to stand overnight at room temperature, then the mixture was concentrated in vacuo. The residue was dissolved in ethanol (10 mL) and ammonium carbonate (335 mg, 3.5 mmol) was added. The reaction mixture was stirred overnight at room temperature then concentrated in vacuo. The residue was purified by preparative thin-layer chromatography (dichloromethane:methanol:NH4OH=5:1:0.1) to yield 113 mg (55%) of the title compound as white crystals. MS (EI) 594.1 (MH+).

后处理

  1. concentrationthe mixture was concentrated in vacuo
  2. dissolutionThe residue was dissolved in ethanol (10 mL)
  3. concentrationthen concentrated in vacuo
  4. customThe residue was purified by preparative thin-layer chromatography (dichloromethane:methanol:NH4OH=5:1:0.1)

来源与证据

ORD记录
ord-7a081a4170fd49858e752668debe463f
来源数据集
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08034827B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记