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

HRID 1445451노트

반응식

HRID 1445451 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-abd27750e5cc4765a1979e34fce0499e
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07666866B2

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