Aluminium lithium hydride → 1-[2-(2-Fluorophenoxy)-ethyl]-4-[3-(3,4,5-trimethoxyphenyl)propyl]-piperazine dihydrochloride

HRID 1928548

反応式

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

参加物

実験手順

To a solution of 1-{4-[2-(2-fluorophenoxy)ethyl]piperazin-1-yl}-3-(3,4,5-trimethoxyphenyl)-propan-1-one hydrochloride (0.2 g, 0.41 mmol) in THF (50 mL) was added LiAlH4 (0.2 g, 5 mmol). The reaction mixture was stirred under N2 for a day, cooled with an ice bath, and quenched with water (0.2 mL) and 10N NaOH aqueous solution (0.2 mL). The solid was filtered and the filtrate was concentrated to dryness. The residue was treated with ether and 2N HCl in ether (2 mL). The white solid was filtered and dried under vacuum to yield the title compound (0.18 g, 87%).

後処理

temperaturecooled with an ice bath
customquenched with water (0.2 mL) and 10N NaOH aqueous solution (0.2 mL)
filtrationThe solid was filtered
concentrationthe filtrate was concentrated to dryness
additionThe residue was treated with ether and 2N HCl in ether (2 mL)
filtrationThe white solid was filtered
customdried under vacuum

出典と根拠

ORDレコード: ord-51b4db710de04d45974849d18197797c
出典データセット: uspto-grants-2012_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08183374B2

反応式

参加物

反応物 2

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート