Water → 2-(4-Benzylpiperazin-2-yl)ethan-1-ol

HRID 1035322ノート

反応式

HRID 1035322 の反応式
[CH2:1]([N:8]1[CH2:13][C:12](=O)[NH:11][C@H:10]([CH2:15][C:16](OCC)=[O:17])[C:9]1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][NH:11][C@H:10]([CH2:15][CH2:16][OH:17])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 91665637HCID 91665637、化合物

生成物 1

HCID 468394992-(4-Benzylpiperazin-2-yl)ethan-1-ol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of Example 255D (9.2 g, 33.3 mmol) in tetrahydrofuran (150 mL) at 0° C. was added lithium aluminum hydride (2 M, tetrahydrofuran, 50 mL) dropwise. The solution was allowed to warm to room temperature and stirred for 16 hours. Water (3.8 mL) in tetrahydrofuran (25 mL) was added dropwise to the solution followed by 3.8 mL NaOH (15% aqueous) and more water (11.4 mL). The solids were removed via filtration. Purification via flash chromatography (0-30% methanol/dichloromethane) afforded the title compound.

後処理

  1. customThe solids were removed via filtration
  2. customPurification via flash chromatography (0-30% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-d1d47afd1173432dbf7f62c8c5112bbd
出典データセット
uspto-grants-2013_10
特許番号
US08546377B2

反応ノート

読み込み中…