Sodium Chloride → HCID 67046038, compound

HRID 1851666Notes

Reaction equation

HRID 1851666 reaction equation
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][N:3]=1.CN[C@H:14]1[CH2:19]N[CH2:17][C@@H:16](NC)[NH:15]1.C(=O)([O-])[O-].[K+].[K+].[Na+].[I-].[Cl-].[Na+].C[N:33]([CH:35]=O)[CH3:34]>>[CH3:19][C@H:14]1[NH:15][C@@H:16]([CH3:17])[CH2:35][N:33]([C:2]2[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][N:3]=2)[CH2:34]1

Participants

7

Reactant 6

HCID 5234Sodium ChlorideHCID 5238Sodium IodideHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 923422-Chloro-5-(trifluoromethyl)pyridineHCID 68313944HCID 68313944, compound

Product 1

HCID 67046038HCID 67046038, compound

Procedure

0.8 g of 2-chloro-5-(trifluoromethyl)pyridine (compound of formula (VII)), 0.5 g of cis-2,6-dimethylaminopiperazine (compound of formula (VI)), 0.67 g of potassium carbonate and 0.3 g of NaI are charged to 8 ml of DMF. The reaction is carried out in a CEM discover microwave initiator for 30 min at 160° C. The resulting product is then poured into a saturated aqueous solution of sodium chloride and the resulting mixture is extracted with ethyl acetate. The organic phase is dried over Na2SO4, filtered and evaporated under vacuum. 1.1 g of an oily material corresponding to the title product are obtained.

Workup

  1. customfor 30 min
  2. customat 160° C
  3. extractionthe resulting mixture is extracted with ethyl acetate
  4. dry with materialThe organic phase is dried over Na2SO4
  5. filtrationfiltered
  6. customevaporated under vacuum

Sources & evidence

ORD record
ord-e8119c28ba4645d3bf77f016cd1e0dd7
Source dataset
uspto-grants-2015_02
Patent number
US08957211B2

Reaction notes

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