Sodium sulfate decahydrate → HCID 12108588, compound

HRID 720329Notes

Reaction equation

HRID 720329 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[NH:8][C:7]([C:16]([N:18]1[CH2:23][CH2:22][N:21]([C:24]([C:26]3[NH:27][C:28]4[C:33]([CH:34]=3)=[CH:32][C:31]([O:35][CH3:36])=[C:30]([O:37][CH3:38])[C:29]=4[O:39][CH3:40])=O)[CH2:20][CH2:19]1)=O)=[CH:6]2.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH3:36][O:35][C:31]1[CH:32]=[C:33]2[C:28](=[C:29]([O:39][CH3:40])[C:30]=1[O:37][CH3:38])[NH:27][C:26]([CH2:24][N:21]1[CH2:20][CH2:19][N:18]([CH2:16][C:7]3[NH:8][C:9]4[C:5]([CH:6]=3)=[CH:4][C:3]([O:2][CH3:1])=[C:11]([O:12][CH3:13])[C:10]=4[O:14][CH3:15])[CH2:23][CH2:22]1)=[CH:34]2

Participants

5

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 21891571HCID 21891571, compound

Product 1

HCID 12108588HCID 12108588, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

N,N′-Bis(5,6,7-trimethoxyindole-2-carbonyl)-piperazine (148 mg) was dissolved in THF (5 mL), and lithium aluminum hydride (10 mg) was gradually added to the solution under ice cooling. The mixture was warmed to room temperature and stirred for 6 hours, and sodium sulfate decahydrate was added thereto. After filtration, the filtrate was concentrated under reduced pressure and purified by column chromatography on silica gel (chloroform:methanol=20:1) to obtain the title compound as a free base.

Workup

  1. filtrationAfter filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. custompurified by column chromatography on silica gel (chloroform:methanol=20:1)

Sources & evidence

ORD record
ord-fbd8690ae742415db0b1cfad790706ea
Source dataset
uspto-grants-2006_11
Patent number
US07135473B2

Reaction notes

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