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

HRID 1916754노트

반응식

HRID 1916754 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a51743834413470dbc11f85107daf55e
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618132B2

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