2-Pyrrolidone → 1-(4-Iodobenzyl)pyrrolidin-2-one

HRID 76155ノート

反応式

HRID 76155 の反応式
[NH:1]1[CH2:5][CH2:4][CH2:3][C:2]1=[O:6].[H-].[Na+].[I:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14]Br)=[CH:12][CH:11]=1>CN(C=O)C>[I:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14][N:1]2[CH2:5][CH2:4][CH2:3][C:2]2=[O:6])=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 120252-PyrrolidoneHCID 24758Sodium hydrideHCID 9542584-Iodobenzyl bromide

生成物 1

HCID 509928621-(4-Iodobenzyl)pyrrolidin-2-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 140 μl (1.68 mmol) 2-pyrrolidone in 5 mL DMF are added 110 mg (2.53 mmol) sodium hydride. Then 500 mg (1.68 mmol) 4-iodobenzyl bromide are added by several portions and the resulting mixture is stirred at r.t. over night. The solvent is removed in vacuo and the residue is resolved in DCM and water. The layers are separated and the organic layer is dried with Na2SO4, filtrated and the solvent is removed in vacuo. The crude product is purified by HPLC.

後処理

  1. customThe solvent is removed in vacuo
  2. customThe layers are separated
  3. dry with materialthe organic layer is dried with Na2SO4
  4. filtrationfiltrated
  5. customthe solvent is removed in vacuo
  6. customThe crude product is purified by HPLC

出典と根拠

ORDレコード
ord-392c23370f18485ea0366c42b5d658a8
出典データセット
uspto-grants-2014_09
特許番号
US08835472B2

反応ノート

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