4-哌啶甲酸 → 1,1'-[Dithiobis(2,1-phenylenecarbonyl)]bis-4-piperidine carboxylic acid

HRID 3738

反应方程式

HRID 3738 反应方程式
[NH:1]1[CH2:9][CH2:8][CH:4]([C:5]([OH:7])=[O:6])[CH2:3][CH2:2]1.[CH3:10][N:11]([Si](C)(C)C)[C:12](=O)[CH3:13].[C:19](Cl)(=[O:37])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[S:26][S:27][C:28]1[CH:36]=[CH:35][CH:34]=[CH:33][C:29]=1[C:30](Cl)=[O:31]>N1C=CC=CC=1.ClCCl>[C:29]1([C:30]([N:11]2[CH2:12][CH2:13][CH:4]([C:5]([OH:7])=[O:6])[CH2:3][CH2:10]2)=[O:31])[CH:33]=[CH:34][CH:35]=[CH:36][C:28]=1[S:27][S:26][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[C:19]([N:1]1[CH2:9][CH2:8][CH:4]([C:5]([OH:7])=[O:6])[CH2:3][CH2:2]1)=[O:37]

参与物

6

反应物 3

HCID 37734-哌啶甲酸HCID 81953N-甲基-N-(三甲基硅基)乙酰胺HCID 881642,2-二硫二苯甲酰氯

产物 1

HCID 189352891,1'-[Dithiobis(2,1-phenylenecarbonyl)]bis-4-piperidine carboxylic acid

试剂、催化剂与溶剂 2

HCID 1049吡啶催化剂HCID 6344二氯甲烷溶剂

实验过程

Isonipecotic acid (4-piperidinecarboxylic acid) (0.76 g, 6 mmol), N-methyl-N-trimethylsilylacetamide and 3 drops of pyridine were stirred at room temperature for 2 hours. This suspension was added to a filtered solution of 2,2'-dithiobisbenzoyl chloride (1.0 g, 3.0 mmol) in 15 mL of dichloromethane. The solvent was removed after 18 hours and the residue was triturated with 1N HCl. The acid was decanted and the residue was dissolved in acetonitrile. After standing for 24 hours a precipitate formed. The solid was collected and dried to give 0.56 g of the title compound, mp>250° C.;

后处理

  1. customThe solvent was removed after 18 hours
  2. customthe residue was triturated with 1N HCl
  3. customThe acid was decanted
  4. dissolutionthe residue was dissolved in acetonitrile
  5. customa precipitate formed
  6. customThe solid was collected
  7. customdried

来源与证据

ORD记录
ord-90022719d27c459586f6b49166817b5d
来源数据集
uspto-grants-1998_03
专利号
US05734081

关联笔记

加载中…