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

HRID 3738

反応式

HRID 3738 の反応式
[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]

参加物

6

反応物 3

HCID 37734-Piperidinecarboxylic acidHCID 81953N-Trimethylsilyl-N-methylacetamideHCID 881642,2'-Dithiodibenzoyl chloride

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

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.;

後処理

  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

出典と根拠

ORDレコード
ord-90022719d27c459586f6b49166817b5d
出典データセット
uspto-grants-1998_03
特許番号
US05734081

関連ノート

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