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

HRID 427657ノート

反応式

HRID 427657 の反応式
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

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18174608HCID 18174608、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2b4ea4ec88934bceb3a58ee33bb2beb6
出典データセット
uspto-grants-2001_11
特許番号
US06313122B1

反応ノート

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