Sodium sulfate decahydrate → HCID 57786003, compound

HRID 1399268Notes

Reaction equation

HRID 1399268 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([C:10]1[CH:15]=[CH:14][C:13]([N:16]2[C:21]3=[N:22][C:23]4[C:24](=[C:25]([C:30](OC)=[O:31])[CH:26]=[CH:27][C:28]=4[Cl:29])[N:20]3[CH2:19][CH2:18][CH2:17]2)=[C:12]([CH3:34])[CH:11]=1)(=[O:9])[NH2:8].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[Cl:29][C:28]1[C:23]2[N:22]=[C:21]3[N:16]([C:13]4[CH:14]=[CH:15][C:10]([C:7]([NH2:8])=[O:9])=[CH:11][C:12]=4[CH3:34])[CH2:17][CH2:18][CH2:19][N:20]3[C:24]=2[C:25]([CH2:30][OH:31])=[CH:26][CH:27]=1

Participants

5

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 57785863HCID 57785863, compound

Product 1

HCID 57786003HCID 57786003, compoundYield 94%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

To a suspension of lithium aluminum hydride (142 mg, 3.74 mmol) in tetrahydrofuran (12 mL) was added a suspension of methyl 1-(4-carbamoyl-2-methylphenyl)-9-chloro-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole-6-carboxylate (500 mg, 1.25 mmol) in tetrahydrofuran (24 mL) at 0° C., and the resultant mixture was stirred at 0° C. for 1 h. After sodium sulfate decahydrate (1.4 g) was added at 0° C., the resultant mixture was filtered and concentrated in vacuo to give the title compound as a yellow solid (433 mg, 1.17 mmol, 94%).

Workup

  1. additionwas added
  2. filtrationthe resultant mixture was filtered
  3. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-8d8402abf3ef4f4185c08016ecc0bc4e
Source dataset
uspto-grants-2014_12
Patent number
US08901141B2

Reaction notes

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