1-Chloro-2-(diethylamine)ethane hydrochloride → N,N-Diethyl-2-[2-(4-phenylbutyl)phenoxy]ethylamine

HRID 743176ノート

反応式

HRID 743176 の反応式
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[OH:17])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].Cl.[CH2:21]([N:23]([CH2:27][CH3:28])[CH2:24][CH2:25]Cl)[CH3:22]>CC(N(C)C)=O>[CH2:21]([N:23]([CH2:27][CH2:28][O:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[CH2:10][CH2:9][CH2:8][CH2:7][C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[CH2:24][CH3:25])[CH3:22]

参加物

5

反応物 3

HCID 133631-Chloro-2-(diethylamine)ethane hydrochlorideHCID 24758Sodium hydrideHCID 125964892-(4-Phenylbutyl)phenol

生成物 1

HCID 19423947N,N-Diethyl-2-[2-(4-phenylbutyl)phenoxy]ethylamine収率 98.2%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

Following a procedure similar to that described in Example 2, 340 mg of 2-(4-phenylbutyl)phenol (prepared as described in Preparation 3), 140 mg of sodium hydride (as a 55% w/w dispersion in mineral oil) and 310 mg of 2-diethylaminoethyl chloride hydrochloride were reacted in 20 ml of dimethylacetamide. The crude product, extracted following the procedure of Example 2, was purified by column chromatography through silica gel, using a 30:1 by volume mixture of methylene chloride and methanol as the eluent, to give 480 mg (yield 98%) of the title compound as an oil.

後処理

  1. extractionThe crude product, extracted
  2. customwas purified by column chromatography through silica gel
  3. additionby volume mixture of methylene chloride and methanol as the eluent

出典と根拠

ORDレコード
ord-fff06daf89d34a47b61ab0946a8c46a9
出典データセット
uspto-grants-1996_09
特許番号
US05556864

反応ノート

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