Acetic Acid → HCID 11644851, compound

HRID 2246900Notes

Reaction equation

HRID 2246900 reaction equation
[NH2:1][C:2]1[C:3]([NH:17][CH3:18])=[C:4]([C:15]#[N:16])[C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2Cl)=[CH:6][CH:7]=1.[ClH:19].[CH3:20][C:21](O)=O>O>[Cl:19][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[C:5]1[CH:6]=[CH:7][C:2]2[N:1]=[C:20]([CH3:21])[N:17]([CH3:18])[C:3]=2[C:4]=1[C:15]#[N:16]

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 68527548HCID 68527548, compound

Product 1

HCID 11644851HCID 11644851, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of 4-Amino-2′-chloro-3-methylamino-biphenyl-2-carbonitrile (intermediate in the preparation of Example 8B) in AcOH (10 mL) and HCl (1 mL) was refluxed for 1 hour. The residue was diluted with water and extracted with AcOEt, and then washed with saturated NaHCO3 aqueous solution. The organics were dried over MgSO4 and the solvent removed in vacuo to give crude product, which used for the next step without further purification. MS (ES) [m+H] calc'd for C16H12ClN3, 281.1; found, 281.1.

Workup

  1. extractionextracted with AcOEt
  2. washwashed with saturated NaHCO3 aqueous solution
  3. dry with materialThe organics were dried over MgSO4
  4. customthe solvent removed in vacuo
  5. customto give crude product, which
  6. customused for the next step without further purification

Sources & evidence

ORD record
ord-cd30a37ba5cf4a618a4d474e5e9cd0ad
Source dataset
uspto-grants-2010_03
Patent number
US07687638B2

Reaction notes

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