Propionic anhydride → HCID 12683866, compound

HRID 235996Notes

Reaction equation

HRID 235996 reaction equation
[NH2:1][C:2]1[N:3]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)[C:4]2[N:5]([CH2:12][CH2:13][N:14]=2)[C:6](=[O:11])[C:7]=1[NH:8][CH:9]=O.[C:23](OC(=O)CC)(=O)[CH2:24]C>N1C=CC=CC=1>[Cl:22][C:19]1[CH:20]=[CH:21][C:16]([CH2:15][N:3]2[C:2]3[N:1]=[C:9]([CH2:23][CH3:24])[NH:8][C:7]=3[C:6](=[O:11])[N:5]3[CH2:12][CH2:13][N:14]=[C:4]23)=[CH:17][CH:18]=1

Participants

4

Procedure

A mixture of 25.00 g. (0.078 mol) of the product of Procedure 2 and 50 ml. dry pyridine in 50 ml. (0.388 mol) of propionic anhydride was heated at reflux for 3 hr. Upon cooling, a white solid precipitated. CH3CN was added, and the white solid filtered and air-dried to give crystals, mp 278.0°-279.0° (corr.). The material may be recrystallized from DMF-i-PrOH.

Workup

  1. additionA mixture of 25.00 g
  2. temperatureat reflux for 3 hr
  3. temperatureUpon cooling
  4. customa white solid precipitated
  5. additionCH3CN was added
  6. filtrationthe white solid filtered
  7. customair-dried
  8. customto give crystals, mp 278.0°-279.0° (corr.)
  9. customThe material may be recrystallized from DMF-i-PrOH

Sources & evidence

ORD record
ord-4214b87ee0c54eac8bf4a44e0e53fa72
Source dataset
uspto-grants-1987_02
Patent number
US04642345

Reaction notes

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