Benzoyl chloride → HCID 57879375、化合物

HRID 1673345ノート

反応式

HRID 1673345 の反応式
C(N(CC)CC)C.[C:8](Cl)(=[O:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[NH2:17][C:18]1[CH:19]=[C:20]([CH:29]=[CH:30][C:31]=1[CH3:32])[C:21]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:22]>C(Cl)Cl>[C:21]([C:20]1[CH:29]=[CH:30][C:31]([CH3:32])=[C:18]([NH:17][C:8](=[O:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:19]=1)(=[O:22])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

参加物

5

反応物 3

HCID 7412Benzoyl chlorideHCID 8471TriethylamineHCID 106085593-Amino-4-methylbenzophenone

生成物 1

HCID 57879375HCID 57879375、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.67 mL of triethylamine and 0.34 ml of benzoyl chloride was added to 5 mL of methylene chloride solution containing 0.51 g of 3-amino-4-methylbenzophenone while ice-cooled and stirred at room temperature for 2 hours. The solvent of the reaction mixture was evaporated under reduced pressure and ethyl acetate and 1.0 mol/L hydrochloric acid were added. The organic layer was separated and dried over anhydrous magnesium sulfate after washed with a saturated sodium hydrogen carbonate aqueous solution and a saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure. Hexane and diisopropyl ether were added to the obtained residue and a solid substance was separated by filtration to obtain 0.71 g of N-(5-benzoyl-2-methylphenyl)benzamide as white solid.

後処理

  1. temperaturecooled
  2. customThe solvent of the reaction mixture was evaporated under reduced pressure and ethyl acetate and 1.0 mol/L hydrochloric acid
  3. additionwere added
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. washafter washed with a saturated sodium hydrogen carbonate aqueous solution
  7. customa saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure
  8. additionHexane and diisopropyl ether were added to the obtained residue
  9. customa solid substance was separated by filtration

出典と根拠

ORDレコード
ord-7848c1e823ca46c282d3059ddb82982e
出典データセット
uspto-grants-2011_08
特許番号
US07999132B2

反応ノート

読み込み中…