Azobisisobutyronitrile → HCID 46899675, compound

HRID 923360Notes

Reaction equation

HRID 923360 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]2[C:11](=[O:12])[O:10][C:8](=[O:9])[C:5]2=[N:6][CH:7]=1.CC(N=NC(C#N)(C)C)(C#N)C.[Cl:25]C1C=CC=CC=1>>[Cl:25][CH2:1][C:2]1[CH:3]=[C:4]2[C:11](=[O:12])[O:10][C:8](=[O:9])[C:5]2=[N:6][CH:7]=1

Participants

4

Reactant 3

HCID 6547AzobisisobutyronitrileHCID 7964ChlorobenzeneHCID 11182791112110-17-5

Product 1

HCID 46899675HCID 46899675, compound

Conditions

Temperature
85 °C

Procedure

106.8 g (0.65 mol) of 5-methyl-2,3-pyridine dicarboxylic acid anhydride were dissolved in 427 g chlorobenzene and heated up to 85° C. A solution of 0.64 g (0.004 mol) AIBN in 99.0 g (0.66 mol) SO2Cl2 was added during 45 min. The mixture was stirred for additional 90 min at 85° C. Chlorobenzene was partly distilled off and the solution was cooled to 10° C. via 10 h ramp. The precipitate was filtered off and washed with chlorobenzene/hexane.

Workup

  1. distillationChlorobenzene was partly distilled off
  2. temperaturethe solution was cooled to 10° C. via 10 h ramp
  3. filtrationThe precipitate was filtered off
  4. washwashed with chlorobenzene/hexane

Sources & evidence

ORD record
ord-2658890c9f1f4c8f89523b3191e3d9c9
Source dataset
uspto-grants-2016_03
Patent number
US09278977B2

Reaction notes

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