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Sodium Iodide → tert-Butyl 9-(pyridin-4-yloxy)-3-azaspiro[5.5]undecane-3-carboxylate

HRID 453911
ノート
印刷プレビュー

反応式

HRID 453911 の反応式
Cl.Cl[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.[H-].[Na+].[OH:11][CH:12]1[CH2:29][CH2:28][C:15]2([CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]2)[CH2:14][CH2:13]1.[I-].[Na+].C([O-])(O)=O.[Na+]>CS(C)=O.CO>[N:6]1[CH:7]=[CH:8][C:3]([O:11][CH:12]2[CH2:13][CH2:14][C:15]3([CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:25])([CH3:26])[CH3:27])=[O:22])[CH2:17][CH2:16]3)[CH2:28][CH2:29]2)=[CH:4][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 5238Sodium IodideHCID 24758Sodium hydrideHCID 818524-Chloropyridine hydrochlorideHCID 516892Sodium BicarbonateHCID 66701044tert-Butyl 9-hydroxy-3-azaspiro[5.5]undecane-3-carboxylate

生成物 1

HCID 66701182tert-Butyl 9-(pyridin-4-yloxy)-3-azaspiro[5.5]undecane-3-carboxylate

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒2 回HCID 887Methanol溶媒

実験手順

4-Chloropyridine hydrochloride (1.3 g) was added to sodium hydride (0.89 g) in DMSO (20 ml), and the mixture was stirred for 10 min. tert-Butyl 9-hydroxy-3-azaspiro[5.5]undecane-3-carboxylate (2.0 g) in DMSO (20 ml) was then added slowly, and the mixture was stirred overnight (TLC monitoring: conversion about 30-35%). A catalytic amount of sodium iodide was added, and the reaction mixture was stirred for 8 h at 80° C. (TLC monitoring). Methanol and NaHCO3 solution were added to the reaction mixture, and stirring was carried out for 20 min. Extraction with ethyl acetate was then carried out, followed by washing with NaHCO3 solution and cold water. The organic phase was dried (Na2SO4) and concentrated under vacuum. The resulting crude product was purified by column chromatography (silica gel, 70% ethyl acetate/hexane). Yield: 1.0 g (40%)

後処理

  1. additionwas then added slowly
  2. stirringthe reaction mixture was stirred for 8 h at 80° C. (TLC monitoring)
  3. stirringstirring
  4. waitwas carried out for 20 min
  5. extractionExtraction with ethyl acetate
  6. washby washing with NaHCO3 solution and cold water
  7. dry with materialThe organic phase was dried (Na2SO4)
  8. concentrationconcentrated under vacuum
  9. customThe resulting crude product was purified by column chromatography (silica gel, 70% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-4759e88456ef49ada152abe2d0d62db1
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492559B2

反応ノート

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