3,3-Diphenylpropylamine → Ethyl (3-{3-[(3,3-diphenylpropyl)amino]propyl}phenoxy)acetate

HRID 2389317노트

반응식

HRID 2389317 반응식
I[CH2:2][CH2:3][CH2:4][C:5]1[CH:6]=[C:7]([CH:15]=[CH:16][CH:17]=1)[O:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11].[C:18]1([CH:24]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:25][CH2:26][NH2:27])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>CN(C=O)C.CCOC(C)=O>[C:28]1([CH:24]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH2:25][CH2:26][NH:27][CH2:2][CH2:3][CH2:4][C:5]2[CH:6]=[C:7]([CH:15]=[CH:16][CH:17]=2)[O:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1

참가 물질

5

반응물 2

HCID 796983,3-DiphenylpropylamineHCID 86637892Ethyl [3-(3-iodopropyl)phenoxy]acetate

생성물 1

HCID 86637891Ethyl (3-{3-[(3,3-diphenylpropyl)amino]propyl}phenoxy)acetate수율 40.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of ethyl [3-(3-iodopropyl)phenoxy]acetate (2.5 g) in DMF (50 mL) was added (3,3-diphenylpropyl)amine (1.7 g) at ambient temperature. The reaction mixture was stirred for 8 hours at the same temperature. The resulting mixture was diluted with EtOAc and washed successively with saturated NaHCO3 aqueous solution, water and brine. The organic layer was dried over anhydrous MgSO4, filtered and evaporated in vacuo. The residue was purified by silica gel column chromatography (chloroform:MeOH=100:0-95:5) to give ethyl (3-{3-[(3,3-diphenylpropyl)amino]propyl}phenoxy)acetate (1.25 g).

후처리

  1. washwashed successively with saturated NaHCO3 aqueous solution, water and brine
  2. dry with materialThe organic layer was dried over anhydrous MgSO4
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customThe residue was purified by silica gel column chromatography (chloroform:MeOH=100:0-95:5)

출처 및 근거

ORD 기록
ord-8483082847264535990166b728b9bbac
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273745B2

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