海萝胶 → HCID 178463795，化合物

HRID 244525

反应方程式

HRID 244525 反应方程式
[CH2:1]([N:3]([CH2:11][CH3:12])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[CH:6][CH:5]=1)[CH3:2].[ClH:13].[CH3:14][N:15]([CH3:27])[C:16]1[CH:17]=[C:18]([NH:22]S(C)(=O)=O)[CH:19]=[CH:20][CH:21]=1.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[K+].[K+]>O.CO>[Cl-:13].[CH2:11]([N:3]([CH2:1][CH3:2])[C:4]1[CH:9]=[CH:8][C:7]2[C:6]([CH:5]=1)=[NH+:22][C:18]1[C:19](=[CH:20][CH:21]=[C:16]([N:15]([CH3:27])[CH3:14])[CH:17]=1)[N:10]=2)[CH3:12]

参与物

7

反应物 4

HCID 313海萝胶2 次HCID 7120N,N-二乙基对苯二胺HCID 24502重铬酸钾HCID 13796402N-[3-(dimethylamino)phenyl]methanesulphonamide

产物 1

HCID 178463795HCID 178463795，化合物收率 22%

试剂、催化剂与溶剂 2

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

实验过程

N,N-diethyl-1,4-phenylenediamine (1.00 g, 6.17 mmol) was added slowly to dilute HCl (700 μl, 32%) in H2O (100 cm3). The mixture was stirred until it was homogeneous. N-[3-(dimethylamino)phenyl]methanesulphonamide (1.32 g, 6.17 mmol) in methanol (60 cm3) was added, followed by a saturated aqueous solution of potassium dichromate (2 cm3). The mixture refluxed for 15 min. The mixture was cooled and diluted with water (200 cm3), acidified with hydrochloric acid (1M) and then extracted with chloroform (6×30 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:9 methanol/dichloromethane) gave the target material as a green solid (451 mg, 22%).

后处理

  1. temperatureThe mixture refluxed for 15 min
  2. temperatureThe mixture was cooled
  3. extractionextracted with chloroform (6×30 cm3)
  4. dry with materialThe combined extracts were dried over sodium sulphate
  5. filtrationfiltered
  6. customthe solvent removed under reduced pressure

来源与证据

ORD记录
ord-62fc057aeeea43c299d1f805d62a92e3
来源数据集
uspto-grants-2014_02
专利号
US08658665B2

关联笔记

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