Pyrrolidine, 2-(2-chloroethyl)-1-methyl-, hydrochloride (1:1) → 1-Methyl-2-(2-{2-[2-(2-methylphenyl)ethyl]phenoxy}ethyl)pyrrolidine

HRID 743295ノート

反応式

HRID 743295 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[OH:16].CC(C)([O-])C.[K+].Cl.Cl[CH2:25][CH2:26][CH:27]1[CH2:31][CH2:30][CH2:29][N:28]1[CH3:32]>CC(N(C)C)=O>[CH3:32][N:28]1[CH2:29][CH2:30][CH2:31][CH:27]1[CH2:26][CH2:25][O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[CH2:9][CH2:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[CH3:1]

参加物

5

反応物 3

HCID 3017050Pyrrolidine, 2-(2-chloroethyl)-1-methyl-, hydrochloride (1:1)HCID 19424010Phenol, 2-[2-(2-methylphenyl)ethyl]-HCID 23665647Potassium tert-butoxide

生成物 1

HCID 194239651-Methyl-2-(2-{2-[2-(2-methylphenyl)ethyl]phenoxy}ethyl)pyrrolidine収率 23%

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), 1.00 g of 2-[2-(2-methylphenyl)ethyl]phenol (prepared as described in Preparation 24), 1.59 g of potassium t-butoxide and 1.73 g of 2-(2-chloroethyl)-1-methylpyrrolidine hydrochloride were reacted in 10 ml of dimethylacetamide. The mixture was then worked up as described in Example 35(a), and the crude product thus obtained was purified by column chromatography through silica gel, using a 10:1 by volume mixture of methylene chloride and methanol as the eluent, to give 350 mg (yield 23%) of the title compound as a solid.

後処理

  1. customthe crude product thus obtained
  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-8815f0d1efe64498a3fc3754840c6380
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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