HCID 178514142, compound → HCID 178508246, compound

HRID 908613Notes

Reaction equation

HRID 908613 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]=[C:4]([OH:12])[C:3]=1[S:13][C:14]#[N:15]>CN(C)C=O.C(OCC)(=O)C>[NH2:15][C:14]1[S:13][C:3]2[C:4]([OH:12])=[N:5][C:6]([C:8]([F:10])([F:11])[F:9])=[N:7][C:2]=2[N:1]=1

Participants

4

Reactant 1

HCID 178514142HCID 178514142, compound

Product 1

HCID 178508246HCID 178508246, compoundYield 78.8%

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 8857Ethyl AcetateSolvent

Procedure

A solution of the compound (4.25 g) obtained in Step 5 in N,N-dimethylformamide (128 ml) was stirred at 130° C. for 14 hr. The reaction mixture was concentrated under reduced pressure, xylene was added to the residue, and the mixture was concentrated again under reduced pressure. The obtained crude crystals were suspended in ethyl acetate, collected by filtration and dried to give the title compound (3.35 g).

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure, xylene
  2. additionwas added to the residue
  3. concentrationthe mixture was concentrated again under reduced pressure
  4. customThe obtained crude crystals
  5. filtrationcollected by filtration
  6. customdried

Sources & evidence

ORD record
ord-7637a417bc314bbb8d39eef083042e03
Source dataset
uspto-grants-2011_09
Patent number
US08017612B2

Reaction notes

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