Ethanol → Dimethylaminoacetaldehyde hydrogen sulphite

HRID 1931206Notes

Reaction equation

HRID 1931206 reaction equation
C([O:3][CH:4](OCC)[CH2:5][N:6]([CH3:8])[CH3:7])C.[S:12](S([O-])=O)([O-:15])(=[O:14])=[O:13].[Na+].[Na+].C(O)C>Cl.O>[CH3:7][N:6]([CH2:5][CH:4]=[O:3])[CH3:8].[S:12]([O-:15])([OH:14])=[O:13]

Participants

6

Reactant 3

HCID 702EthanolHCID 77163(2,2-Diethoxyethyl)dimethylamineHCID 656671Sodium Pyrosulfite

Product 1

HCID 86636908Dimethylaminoacetaldehyde hydrogen sulphite

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolventHCID 962WaterSolvent2×

Procedure

40 g of dimethylaminoacetaldehyde diethylacetal are heated to 40° C. in a mixture of 48 g conc. hydrochloric acid and 20 ml of water for 3 h. Then a solution of 42.4 g sodium pyrosulphite in 72 ml of water (sodium hydrogen sulphite solution) is added dropwise and the mixture is stirred for 1 h. 200 ml of ethanol are added and then the mixture is stirred for 2 h at 0° C. The suspension is suction filtered, washed with 160 ml of ethanol and dried at 45° C. in vacuo.

Workup

  1. stirringthe mixture is stirred for 2 h at 0° C
  2. filtrationsuction filtered
  3. washwashed with 160 ml of ethanol
  4. customdried at 45° C. in vacuo

Sources & evidence

ORD record
ord-60c0c9ef33024fba81c0240e7cced895
Source dataset
uspto-grants-2012_05
Patent number
US08188274B2

Reaction notes

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