Isopropanol → HCID 86736720, compound

HRID 1447617Notes

Reaction equation

HRID 1447617 reaction equation
[C:1]([O-:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([O-:6])=[O:5].[CH3:9][CH:10]([OH:12])[CH3:11].C(OCC)(=O)C.C(O)(=O)/C=C\C(O)=O>C(OCC)C>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][CH:10]([OH:12])[CH3:11]

Participants

6

Reactant 4

HCID 3776IsopropanolHCID 8857Ethyl AcetateHCID 444266Maleic AcidHCID 5288227Maleate(2-)

Product 1

HCID 86736720HCID 86736720, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

This example illustrates methods of preparing the maleate addition salts of compounds of formula (I)A. In this example, one gram of 1-isopropylamino-3-(4-[2-(endobicyclo[3.1.0]hex-6-yl)ethylureido]-1-phenoxy)-2-propanol is dissolved in 5 ml. of ethyl acetate at 20° C. To this solution is added 10 ml. of a saturated solution of maleic acid in ethyl ether. The mixture is allowed to stand for one hour at room temperature. The resulting precipitate is recovered by filtration, washed three times with ethyl ether and then crystallized from a mixture of ethyl ether and ethanol (10:1) affording crystalline 1-isopropylamino-3-(4-[2-(endobicyclo[3.1.0]hex-6-yl)ethylureido]-1-phenoxy)-2-propanol maleate.

Workup

  1. custommethods of preparing
  2. customat 20° C
  3. additionTo this solution is added 10 ml
  4. filtrationThe resulting precipitate is recovered by filtration
  5. washwashed three times with ethyl ether
  6. customcrystallized from a mixture of ethyl ether and ethanol (10:1)

Sources & evidence

ORD record
ord-25ebd06959ef49b3a5029e2ce2f4580b
Source dataset
uspto-grants-1979_12
Patent number
US04177280

Reaction notes

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