Sodium Hydroxide → 2,3-Bis[(4-methoxybenzoyl)amino]phenol

HRID 395807노트

반응식

HRID 395807 반응식
COC1C=CC(C(O[O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([NH:17][C:18](=[O:27])[C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)[C:12]=2[NH:28][C:29](=[O:38])[C:30]2[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][CH:31]=2)=O)=CC=1.[OH-].[Na+]>CO>[CH3:37][O:36][C:33]1[CH:32]=[CH:31][C:30]([C:29]([NH:28][C:12]2[C:13]([NH:17][C:18](=[O:27])[C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)=[CH:14][CH:15]=[CH:16][C:11]=2[OH:10])=[O:38])=[CH:35][CH:34]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 18174608HCID 18174608, 화합물

생성물 1

HCID 106442072,3-Bis[(4-methoxybenzoyl)amino]phenol수율 40%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 2,3-bis[(4-methoxybenzoyl)amino]phenoxy 4-methoxybenzoate (7.75 g, 14.7 mmol) in methanol (100 mL) was cooled to ice-water bath temperature and 5 N aqueous sodium hydroxide solution (3.0 mL) was added. The reaction mixture was allowed to warm to room temperature and stirred for 72 hr. The reaction mixture was concentrated in vacuo and the resulting solid was dissolved in methylene chloride and washed with dilute aqueous hydrochloric acid, water, and saturated sodium chloride solution. The organic layer was dried (sodium sulfate), filtered, and concentrated in vacuo. Recrystallization of the residue from diethyl ether/hexane gave 2.3 g (40%) of the title product. mp 208-209° C.

후처리

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionthe resulting solid was dissolved in methylene chloride
  4. washwashed with dilute aqueous hydrochloric acid, water, and saturated sodium chloride solution
  5. dry with materialThe organic layer was dried (sodium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customRecrystallization of the residue from diethyl ether/hexane

출처 및 근거

ORD 기록
ord-44301514b7b2450687753a7b1982651e
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06605626B2

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