4-Iodophenol → 1-(2-(4-Iodophenoxy)ethyl)pyrrolidine

HRID 1916754ノート

反応式

HRID 1916754 の反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.Cl.Cl[CH2:11][CH2:12][N:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[I:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:11][CH2:12][N:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 108944-IodophenolHCID 11430Potassium CarbonateHCID 816681-(2-Chloroethyl)pyrrolidine hydrochloride

生成物 1

HCID 219591661-(2-(4-Iodophenoxy)ethyl)pyrrolidine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A reaction mixture of 44 g (0.2 mol) 4-iodophenol, 34 g (0.2 mol) 1-(2-chloro-ethyl)-pyrrolidine-hydrochloride, 110.56 g (0.8 mol) K2CO3 and 800 mL DMF is stirred for 48 h at RT. The reaction mixture is filtered and the filtrate is evaporated down. The residue is taken up in water and extracted with EtOAc. The organic phase is extracted with saturated NaCl solution and dried over Na2SO4. The purification is carried out by column chromatography on silica gel (EtOAc/MeOH/NH3 85:15:1.5).

後処理

  1. filtrationThe reaction mixture is filtered
  2. customthe filtrate is evaporated down
  3. extractionextracted with EtOAc
  4. extractionThe organic phase is extracted with saturated NaCl solution
  5. dry with materialdried over Na2SO4
  6. customThe purification

出典と根拠

ORDレコード
ord-a51743834413470dbc11f85107daf55e
出典データセット
uspto-grants-2013_12
特許番号
US08618132B2

反応ノート

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