Hydrochloric Acid → HCID 18765562, compound

HRID 480590Notes

Reaction equation

HRID 480590 reaction equation
[C:1]([O:5][C:6](=[O:14])[CH2:7][NH:8][C:9]([CH3:13])([CH3:12])[CH2:10][OH:11])(C)(C)[CH3:2].[ClH:15].C(OCC)(=O)C.CO>C(O)C>[ClH:15].[CH2:1]([O:5][C:6](=[O:14])[CH2:7][NH:8][C:9]([CH3:13])([CH3:12])[CH2:10][OH:11])[CH3:2]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 18765574HCID 18765574, compoundHCID 21584119Ethylacetate methanol

Product 1

HCID 18765562HCID 18765562, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

63.00 g of tert-butyl(2-hydroxy-1,1-dimethylethylamino)acetate are placed in 500 ml of ethanol. Then, while cooling with an ice bath, about 200 g of hydrogen chloride are introduced over a period of about four hours. The reaction mixture is stirred overnight at ambient temperature. For working up, it is concentrated by evaporation and stirred with toluene. Then the toluene is distilled off. A viscous oil remains, which is reacted further without any additional purification. Rf value: 0.16 (silica gel, ethyl acetate/methanol=9:1); mass spectrum (ESI+): m/z=176 [M+H]+.

Workup

  1. temperatureThen, while cooling with an ice bath
  2. concentrationit is concentrated by evaporation
  3. stirringstirred with toluene
  4. distillationThen the toluene is distilled off
  5. customA viscous oil remains, which is reacted further without any additional purification

Sources & evidence

ORD record
ord-2477550a52d5421086634e2d9b9fc7da
Source dataset
uspto-grants-2003_11
Patent number
US06653305B2

Reaction notes

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