Sodium sulfate decahydrate → HCID 57786347, compound

HRID 1399243Notes

Reaction equation

HRID 1399243 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[N:7]([CH:10]1[CH2:19][N:18]2[C:14](=[N:15][C:16]3[C:17]2=[C:20]([N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])[CH:21]=[CH:22][CH:23]=3)[N:13]([C:29]2[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][C:30]=2[Cl:36])[CH2:12][CH2:11]1)=[N+]=[N-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[Cl:36][C:30]1[CH:31]=[C:32]([Cl:35])[CH:33]=[CH:34][C:29]=1[N:13]1[C:14]2=[N:15][C:16]3[C:17](=[C:20]([N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])[CH:21]=[CH:22][CH:23]=3)[N:18]2[CH2:19][CH:10]([NH2:7])[CH2:11][CH2:12]1

Participants

5

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 57785923HCID 57785923, compound

Product 1

HCID 57786347HCID 57786347, compoundYield 75.2%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

To a suspension of lithium aluminum hydride (31.8 mg, 0.858 mmol) in tetrahydrofuran (1 mL) was added a solution of 4-azido-1-(2,4-dichlorophenyl)-N,N-diethyl-2,3,4,5-tetrahydro-1H-[1,3]diazepino[1,2-a]benzimidazol-7-amine (95.0 mg, 0.214 mmol) in tetrahydrofuran (1 mL) at 0° C. After the resultant mixture was stirred at 0° C. for 2 hr, sodium sulfate decahydrate (320 mg) was added. The resultant mixture was filtered and concentrated in vacuo. The residue was recrystallized from ethyl acetate/diisopropyl ether to give the title compound as a colorless solid (67.2 mg, 0.161 mmol, 75%).

Workup

  1. filtrationThe resultant mixture was filtered
  2. concentrationconcentrated in vacuo
  3. customThe residue was recrystallized from ethyl acetate/diisopropyl ether

Sources & evidence

ORD record
ord-ee2b367e56e94380a5716bcd26ac50fc
Source dataset
uspto-grants-2014_12
Patent number
US08901141B2

Reaction notes

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