Potassium Carbonate → HCID 22769491, compound

HRID 258757Notes

Reaction equation

HRID 258757 reaction equation
C(O)(=O)C([O:4][CH:5]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH2:6][NH:7][CH:8]([CH3:20])[CH2:9][NH:10][C:11](=[O:19])[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=O.C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C>[CH3:20][CH:8]([NH:7][CH2:6][CH:5]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[OH:4])[CH2:9][NH:10][C:11](=[O:19])[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 131710098HCID 131710098, compound

Product 1

HCID 22769491HCID 22769491, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

A mixture of 3.8 g. of 2-(1-methyl-2-phenylacetamidoethyl)amino-1-phenylethanol hydrogen oxalate (m.p. 160°-161° C.; Example 4) is stirred with 50 ml. of 10% aqueous potassium carbonate solution and 50 ml. of ethyl acetate. The ethyl acetate phase is separated, dried over anhydrous magnesium sulphate, and evaporated to dryness under reduced pressure. The residue is crystallised four times from 20 ml. of toluene each time. There is thus obtained one specific diastereoisomer (Isomer A) of 2-(1-methyl-2-phenylacetamidoethyl)amino-1-phenylethanol, m.p. 100°-101° C.

Workup

  1. additionA mixture of 3.8 g
  2. customThe ethyl acetate phase is separated
  3. dry with materialdried over anhydrous magnesium sulphate
  4. customevaporated to dryness under reduced pressure
  5. customThe residue is crystallised four times from 20 ml

Sources & evidence

ORD record
ord-f1c675e68af44691bfd183c15d94b980
Source dataset
uspto-grants-1977_07
Patent number
US04034112

Reaction notes

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