Diethyl Ether → HCID 21993943, compound

HRID 1978454Notes

Reaction equation

HRID 1978454 reaction equation
[CH2:1]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([CH2:15][CH2:16][CH2:17][NH:18][C:19]([C:21]2[S:31][C:30]3[N:32]4[C:23](=[CH:24][N:25]=[C:26]4[CH:27]=[CH:28][CH:29]=3)[CH:22]=2)=[O:20])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:33].C(OCC)(=O)C.CCOCC>C(O)C>[ClH:33].[ClH:33].[ClH:33].[CH2:1]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([CH2:15][CH2:16][CH2:17][NH:18][C:19]([C:21]2[S:31][C:30]3[N:32]4[C:23](=[CH:24][N:25]=[C:26]4[CH:27]=[CH:28][CH:29]=3)[CH:22]=2)=[O:20])[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 21866389Hydrogen chloride-ethyl acetateHCID 21993944HCID 21993944, compound

Product 1

HCID 21993943HCID 21993943, compoundYield 94%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 320.0 mg (0.71 mM) of N-[3-(4-benzyl-2,3,5,6-tetrahydro-7H-1,4-diazepin-1-yl)propan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added 2 ml (8.0 mM) of 4N-HCl/ethyl acetate, and the mixture was stirred under heating for 2 hours. To the ethanolic solution containing crystals was added ether and the crystal crop was harvested by filtration and rinsed with ethanol and diethyl ether to provide the title compound as light-orange-colored crystals (390.9 mg, 94%).

Workup

  1. temperatureunder heating for 2 hours
  2. additionTo the ethanolic solution containing crystals
  3. filtrationthe crystal crop was harvested by filtration
  4. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-dd2785faba254438baf7ea4e5b51828e
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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