Sodium Pyrosulfite → HCID 86614376, compound

HRID 1817794Notes

Reaction equation

HRID 1817794 reaction equation
[CH3:1][N:2]([CH2:9][CH2:10][O:11][C:12]1[CH:19]=[CH:18][C:15]([CH:16]=[O:17])=[CH:14][CH:13]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[S:20]([S:24]([O-:26])=[O:25])([O-:23])(=[O:22])=[O:21].[Na+:27].[Na+]>O>[S:20]([S:24]([O-:26])=[O:25])([O-:23])(=[O:22])=[O:21].[Na+:27].[CH3:1][N:2]([CH2:9][CH2:10][O:11][C:12]1[CH:13]=[CH:14][C:15]([CH:16]=[O:17])=[CH:18][CH:19]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[Na+:27]

Participants

4

Reactant 2

HCID 656671Sodium PyrosulfiteHCID 104225464-{2-[Methyl(pyridin-2-yl)amino]ethoxy}benzaldehyde

Product 1

HCID 86614376HCID 86614376, compoundYield 77.4%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
15 °C

Procedure

4-[2-(N-methyl-N-(2-pyridyl)amino)ethoxy]benzaldehyde (10 gms, 0.039M) was stirred with industrial spirit (150 ml) and cooled to 15° C. A solution of sodium metabisulphite (11 gms, 0.057M) in water (20 ml) was added drop wise to the above solution over a time period of about 15 to 20 minutes, whilst maintaining the temperature below about 20° C. The reaction mixture was further cooled to 10° C. and stirred for 1 to 2 hours. The resulting precipitate was then filtered and washed with industrial spirit (25 ml×2) followed by water (25 ml). The solid obtained was then dried in a vacuum oven at 40° C. to obtain the title complex (10 gms, HPLC purity 98.5%).

Workup

  1. temperaturewhilst maintaining the temperature below about 20° C
  2. temperatureThe reaction mixture was further cooled to 10° C.
  3. filtrationThe resulting precipitate was then filtered
  4. washwashed with industrial spirit (25 ml×2)
  5. customThe solid obtained
  6. customwas then dried in a vacuum oven at 40° C.

Sources & evidence

ORD record
ord-01f1e0e39e774832abd4d64e8c946966
Source dataset
uspto-grants-2009_10
Patent number
US07598387B2

Reaction notes

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