Potassium Carbonate → HCID 21081033, compound

HRID 1965940Notes

Reaction equation

HRID 1965940 reaction equation
[C:1]([NH:4][CH2:5][CH2:6][NH2:7])(=[O:3])[CH3:2].[Cl:8][C:9]1[N:14]=[C:13](Cl)[C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][N:10]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[Cl:8][C:9]1[N:10]=[C:11]([NH:7][CH2:6][CH2:5][NH:4][C:1](=[O:3])[CH3:2])[C:12]([C:16]([F:19])([F:17])[F:18])=[CH:13][N:14]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 66082N-(2-aminoethyl)acetamideHCID 27827742,4-Dichloro-5-(trifluoromethyl)pyrimidine

Product 1

HCID 21081033HCID 21081033, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

1.84 g of 2-acetylamino-ethylamine dissolved in 10 ml of dioxane are added to 3.91 g of 2,4-dichloro-5-trifluoromethyl-pyrimidine in 20 ml dioxane at ambient temperature. Then 3.7 ml of 5 M potassium carbonate solution are added and the mixture is stirred for three days at ambient temperature. It is then filtered through Alox B and washed with dioxane. The filtrate is concentrated by evaporation and the residue separated by chromatography through a silica gel column with cyclohexane:ethyl acetate:methanol (5:4:1).

Workup

  1. filtrationIt is then filtered through Alox B
  2. washwashed with dioxane
  3. concentrationThe filtrate is concentrated by evaporation
  4. customthe residue separated by chromatography through a silica gel column with cyclohexane:ethyl acetate:methanol (5:4:1)

Sources & evidence

ORD record
ord-d31f87e0aba7439db0c90785b791a560
Source dataset
uspto-grants-2013_04
Patent number
US08420630B2

Reaction notes

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