Ammonia → HCID 57194161, compound

HRID 1901169

Reaction equation

HRID 1901169 reaction equation
C[O:2][C:3]([CH2:5][C:6]1[CH:26]=[CH:25][C:9]([O:10][CH2:11][CH:12]([NH:14][CH2:15][CH:16]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[CH:19]=2)[OH:17])[CH3:13])=[C:8]([Cl:27])[CH:7]=1)=O.[NH3:28]>CO>[C:3]([CH2:5][C:6]1[CH:26]=[CH:25][C:9]([O:10][CH2:11][CH:12]([NH:14][CH2:15][CH:16]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[CH:19]=2)[OH:17])[CH3:13])=[C:8]([Cl:27])[CH:7]=1)(=[O:2])[NH2:28]

Participants

4

Reactant 2

HCID 222AmmoniaHCID 218321762-[2-(4-Methoxycarbonylmethyl-2-chlorophenoxy)-1-methylethyl]amino-1-(3-chlorophenyl)ethanol

Product 1

HCID 57194161HCID 57194161, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 2 g of 2-[2-(4-methoxycarbonylmethyl-2-chlorophenoxy) -1-methylethyl]amino-1-(3-chlorophenyl)ethanol (prepared as described in Example 22) dissolved in 50 ml of methanol was saturated with gaseous ammonia in a reaction vessel, whilst ice-cooling, after which the reaction vessel was tightly stoppered and allowed to stand at room temperature for one week. At the end of this time, the solvent (methanol) was removed by distillation under reduced pressure, and the residue was recrystallized from ethyl acetate, to give 0.55 g of the title compound as crystals, melting at 99°-101° C.

Workup

  1. temperaturecooling
  2. waitto stand at room temperature for one week
  3. customAt the end of this time, the solvent (methanol) was removed by distillation under reduced pressure
  4. customthe residue was recrystallized from ethyl acetate

Sources & evidence

ORD record
ord-c4979ee582e84021838b5db0b01330d9
Source dataset
uspto-grants-1996_11
Patent number
US05576340

Linked notes

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