Hydrochloric Acid → N1-(4-methoxybenzoyl)-N2-(2-naphthoyl)-benzenediamine

HRID 395701

反応式

HRID 395701 の反応式
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]([C:7]([NH:9][C:10]2[C:11]([NH2:16])=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:8])=[CH:5][CH:4]=1.N1C=CC=CC=1.[CH:25]1[C:34]2[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=2)[CH:28]=[CH:27][C:26]=1[C:35](Cl)=[O:36].Cl>C(Cl)(Cl)Cl.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([NH:9][C:10]2[C:11]([NH:16][C:35]([C:26]3[CH:27]=[CH:28][C:29]4[C:34](=[CH:33][CH:32]=[CH:31][CH:30]=4)[CH:25]=3)=[O:36])=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:8])=[CH:17][CH:18]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 752462-Naphthoyl chlorideHCID 785232N-(2-Aminophenyl)-4-methoxybenzamide

生成物 1

HCID 21352792N1-(4-methoxybenzoyl)-N2-(2-naphthoyl)-benzenediamine収率 65%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of N1-(4-methoxybenzoyl)-1,2-benzenediamine (200 mg, 0.826 mmol) and pyridine (0.25 mL) in chloroform (5 mL) was treated with 2-naphthoyl chloride (158 mg, 0.826 mmol). After 20 h, the mixture was poured into a mixture of ethyl acetate and 1 N aqueous hydrochloric acid. The organic layer was washed with water, saturated sodium chloride solution, and dried (potassium carbonate), filtered, and concentrated in vacuo. Recrystallization from hexanes/ethyl acetate yielded 211 mg (65%) of the title compound.

後処理

  1. washThe organic layer was washed with water, saturated sodium chloride solution
  2. dry with materialdried (potassium carbonate)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customRecrystallization from hexanes/ethyl acetate

出典と根拠

ORDレコード
ord-610667b255af48dfb5d730a62b4d12e7
出典データセット
uspto-grants-2003_08
特許番号
US06605626B2

関連ノート

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