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

HRID 2389317ノート

反応式

HRID 2389317 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-8483082847264535990166b728b9bbac
出典データセット
uspto-grants-2012_09
特許番号
US08273745B2

反応ノート

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