Pyrrolidine, 2-(2-chloroethyl)-1-methyl-, hydrochloride (1:1) → 2-(2-{2-[2-(3-Methoxymethoxyphenyl)ethyl]phenoxy}ethyl]-1-methylpyrrolidin

HRID 743252ノート

反応式

HRID 743252 の反応式
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[OH:19])[CH:8]=[CH:9][CH:10]=1.CC(C)([O-])C.[K+].Cl.Cl[CH2:28][CH2:29][CH:30]1[CH2:34][CH2:33][CH2:32][N:31]1[CH3:35]>CC(N(C)C)=O>[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[O:19][CH2:28][CH2:29][CH:30]2[CH2:34][CH2:33][CH2:32][N:31]2[CH3:35])[CH:8]=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 3017050Pyrrolidine, 2-(2-chloroethyl)-1-methyl-, hydrochloride (1:1)HCID 194238312-[2-(3-Methoxymethoxyphenyl)ethyl]phenolHCID 23665647Potassium tert-butoxide

生成物 1

HCID 194238962-(2-{2-[2-(3-Methoxymethoxyphenyl)ethyl]phenoxy}ethyl]-1-methylpyrrolidin収率 62%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

Following a procedure similar to that described in Example 35(a), 2.37 g of 2-[2-(3-methoxymethoxyphenyl)ethyl]phenol (prepared as described in Preparation 21), 1.03 g of potassium t-butoxide and 1.69 g of 2-(2-chloroethyl)-1-methylpyrrolidine hydrochloride were reacted in 50 ml of dimethylacetamide. The reaction mixture was then worked up as described in Example 35(a), and the crude product was purified by column chromatography through silica gel, using a 20:1 by volume mixture of methylene chloride and methanol as the eluent, to give 1.87 g (yield 62%) of the title compound as a colorless oil.

後処理

  1. customthe crude product was purified by column chromatography through silica gel
  2. additionby volume mixture of methylene chloride and methanol as the eluent

出典と根拠

ORDレコード
ord-e57a6f532cd94ad2914919b13c27bbda
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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