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

HRID 395701

반응식

HRID 395701 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-610667b255af48dfb5d730a62b4d12e7
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06605626B2

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