Sodium sulfate decahydrate → HCID 66819253, compound

HRID 1617147Notes

Reaction equation

HRID 1617147 reaction equation
C([O:3][C:4](=O)[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH2:11][C:12]2[C:13]([CH3:25])=[N:14][C:15]([NH2:24])=[N:16][C:17]=2[NH:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[CH:6]=1)C.[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>[NH2:24][C:15]1[N:14]=[C:13]([CH3:25])[C:12]([CH2:11][C:7]2[CH:6]=[C:5]([CH2:4][OH:3])[CH:10]=[CH:9][CH:8]=2)=[C:17]([NH:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[N:16]=1

Participants

5

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 66819205HCID 66819205, compound

Product 1

HCID 66819253HCID 66819253, compoundYield 97.2%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

A solution of the product from step (iii) (0.7 g) in THF (10 mL) was added to a solution of lithium aluminium hydride (1M in THF, 4.1 mL) in THF (10 mL) at 0° C. The mixture was stirred at rt for 2 h, sodium sulfate decahydrate (10 g) was added and the suspension stirred for 1 h. The suspension was filtered and the filtrate diluted with saturated aq ammonium chloride (20 mL). The aqueous phase was separated and the organic phase dried and evaporated under reduced pressure to give the subtitle compound 0.60 g, which was used without further purification.

Workup

  1. stirringthe suspension stirred for 1 h
  2. filtrationThe suspension was filtered
  3. additionthe filtrate diluted with saturated aq ammonium chloride (20 mL)
  4. customThe aqueous phase was separated
  5. customthe organic phase dried
  6. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-5c0203d685fe4a20aa56dcd78933d2d5
Source dataset
uspto-grants-2014_07
Patent number
US08765939B2

Reaction notes

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