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

HRID 3738

반응식

HRID 3738 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 1049Pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.;

후처리

  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

출처 및 근거

ORD 기록
ord-90022719d27c459586f6b49166817b5d
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05734081

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