Aminoacetaldehyde dimethyl acetal → HCID 54527212, compound

HRID 1975025Notes

Reaction equation

HRID 1975025 reaction equation
[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][NH2:5].[CH:8](=O)/[CH:9]=[CH:10]/[CH3:11]>C(O)C>[CH2:8]([NH:5][CH2:4][CH:3]([O:6][CH3:7])[O:2][CH3:1])[CH:9]=[CH:10][CH3:11]

Participants

4

Conditions

Temperature
0 °C

Procedure

200 g of molecular sieve are initially introduced into 1000 ml of ethanol, and 105 g (1 mol) of aminoacetaldehyde dimethyl acetal and 70 g (1 mol) of crotonaldehyde are added. The mixture is allowed to stand overnight at room temperature, the liquid phase is decanted off from the molecular sieve and cooled to 0° C., and 40 g of sodium borohydride are added in 1 g portions. The mixture is subsequently stirred overnight at room temperature and concentrated, the concentrate is taken up in 500 ml of water, and the potassium carbonate is added until an organic phase separates off. The mixture is extracted using chloroform, and the extract is dried over potassium carbonate, concentrated and distilled.

Workup

  1. additionare added
  2. customthe liquid phase is decanted off from the molecular sieve
  3. addition40 g of sodium borohydride are added in 1 g portions
  4. waitThe mixture is subsequently stirred overnight at room temperature
  5. concentrationconcentrated
  6. additionthe potassium carbonate is added until an organic phase
  7. extractionThe mixture is extracted
  8. dry with materialthe extract is dried over potassium carbonate
  9. concentrationconcentrated
  10. distillationdistilled

Sources & evidence

ORD record
ord-506d6cd4cb334fca878166cb60016216
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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