Ammonia → (4-(2-(Azepan-1-yl)ethoxy)phenyl)methanol

HRID 1433806ノート

反応式

HRID 1433806 の反応式
C([O:3][C:4](=O)[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][N:14]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)=[CH:7][CH:6]=1)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].N>O1CCCC1>[N:14]1([CH2:13][CH2:12][O:11][C:8]2[CH:7]=[CH:6][C:5]([CH2:4][OH:3])=[CH:10][CH:9]=2)[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

参加物

5

反応物 3

HCID 222AmmoniaHCID 21226445Aluminium lithium hydrideHCID 66625442HCID 66625442、化合物

生成物 1

HCID 9816367(4-(2-(Azepan-1-yl)ethoxy)phenyl)methanol収率 70.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 4-(2-azepan-1-ylethoxy)benzoic acid ethyl ester (6.0 g) in tetrahydrofuran (60 ml) was added lithium aluminum hydride (1.5 g) under a nitrogen atmosphere, the solution was stirred overnight at room temperature, tetrahydrofuran and aqueous ammonia were then sequentially added thereto on an ice bath, the solution was filtered through celite pad, the solvent was evaporated in vacuo to provide [4-(2-azepan-1-ylethoxy)phenyl]methanol (3.6 g). The title compound (194 mg) was obtained according to an analogous synthetic method to Preparation Example 13 using the above compound (200 mg).

後処理

  1. filtrationon an ice bath, the solution was filtered through celite pad
  2. customthe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-58c76842a7904c09bbab56a9db8465b4
出典データセット
uspto-grants-2009_11
特許番号
US07612114B2

反応ノート

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