Trioxifene → [2-(4-Methoxyphenyl)-3,4-dihydronaphth-1-yl][4-(1-pyrrolidinyl-2-ethoxy)phenyl]carbinol

HRID 399443

反応式

HRID 399443 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:18][CH2:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]=2[C:19]([C:21]2[CH:26]=[CH:25][C:24]([O:27][CH2:28][CH2:29][N:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)=[CH:23][CH:22]=2)=[O:20])=[CH:5][CH:4]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:18][CH2:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]=2[CH:19]([C:21]2[CH:26]=[CH:25][C:24]([O:27][CH2:28][CH2:29][N:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)=[CH:23][CH:22]=2)[OH:20])=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 50139TrioxifeneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 10182739[2-(4-Methoxyphenyl)-3,4-dihydronaphth-1-yl][4-(1-pyrrolidinyl-2-ethoxy)phenyl]carbinol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

850 mg (1.9 mmol) of [2-(4-methoxyphenyl)-3,4-dihydronaphth-1-yl][4-(1-pyrrolidinyl-2-ethoxy)phenyl] methanone was dissolved in 100 mL of THF and 160 mg (4 mmol) of LiAlH4 was added. The reaction mixture was stirred at room temperature and under a N2 atmosphere for eighteen hours. The reaction mixture was evaporated to dryness in vacuo. Fifty mL of water was carefully added to the residue and the reaction mixture was extracted twice with 100 mL of EtOAc. The EtOAc extracts were combind and washed with water, then the EtOAc layer was removed and dried by filteration through anhydrous Na2SO4 and evaporated to dryness in vacuo. This yielded 670 mg of the title compound as a white amorphous powder.

後処理

  1. customThe reaction mixture was evaporated to dryness in vacuo
  2. additionFifty mL of water was carefully added to the residue
  3. extractionthe reaction mixture was extracted twice with 100 mL of EtOAc
  4. washwashed with water
  5. customthe EtOAc layer was removed
  6. dry with materialdried by filteration through anhydrous Na2SO4
  7. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-0c6825c12e8446f98cbbe66ea9902b83
出典データセット
uspto-grants-1998_10
特許番号
US05821253

関連ノート

読み込み中…