Water → N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine

HRID 1445451ノート

反応式

HRID 1445451 の反応式
FC(F)(F)C(O)=O.[NH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:37]=[C:36]([O:38][CH3:39])[CH:35]=[CH:34][C:13]=1[C:14]([NH:16][C:17]1[C:18]([NH:23][C:24](=[O:33])[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:19][CH:20]=[CH:21][CH:22]=1)=[O:15].O.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[NH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:37]=[C:36]([O:38][CH3:39])[CH:35]=[CH:34][C:13]=1[C:14]([NH:16][C:17]1[C:18]([NH:23][C:24](=[O:33])[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:19][CH:20]=[CH:21][CH:22]=1)=[O:15]

参加物

5

反応物 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 86628410N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine trifluoroacetate

生成物 1

HCID 86628411N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine収率 85%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

The free base form of N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine was prepared by vigorously stirring N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine trifluoroacetate (1.88 g, 3.42 mmol) with 100 ml water, 2 grams potassium carbonate and 100 ml of CH2Cl2 for several hours at room temperature. After stirring, the organic layer was set aside and combined with a 150 ml CH2Cl2 wash of the original aqueous layer. The combined CH2Cl2 extracts were washed with brine, dried over Na2SO4, concentrated in vacuo, then purified on a chromatotron system (4 mm plate) with 9:1 CH2Cl2:MeOH eluent to provide N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine (1.26 g, 85%) as a brittle white foam after high vacuum drying.

後処理

  1. washwash of the original aqueous layer
  2. washThe combined CH2Cl2 extracts were washed with brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. custompurified on a chromatotron system (4 mm plate) with 9:1 CH2Cl2

出典と根拠

ORDレコード
ord-abd27750e5cc4765a1979e34fce0499e
出典データセット
uspto-grants-2010_02
特許番号
US07666866B2

反応ノート

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