Cesium carbonate → 2-Chloro-5-(2,2-dimethylpropoxy)pyridine

HRID 242242ノート

反応式

HRID 242242 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.I[CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12].C(=O)([O-])[O-].[Cs+].[Cs+]>COCCOCCOC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[CH:6][N:7]=1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 84953Propane, 1-iodo-2,2-dimethyl-HCID 8198212-Chloro-5-hydroxypyridine

生成物 1

HCID 592802202-Chloro-5-(2,2-dimethylpropoxy)pyridine

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

実験手順

5.2 g (40.0 mmol) 6-chloropyridin-3-ol, 11.9 g (60.0 mmol) 1-iodo-2,2-dimethylpropane, 19.6 g (60.0 mmol) cesium carbonate and 120 ml diethylene glycol dimethyl ether are divided into five portions of equal size and are reacted in portions at 160° C. for 4 h in a single mode microwave (CEM Explorer). Thereafter, the five reaction mixtures obtained are combined, the solid is filtered off and rinsed with diethylene glycol dimethyl ether and the filtrate and wash solutions are combined. The majority of the solvent is removed and 300 ml water are added to the concentrated solution (approx. 50 ml). The mixture is stirred for 30 min and the solid obtained is filtered off, washed once with water and dried under a high vacuum.

後処理

  1. customare reacted in portions at 160° C. for 4 h in a single mode microwave (CEM Explorer)
  2. customThereafter, the five reaction mixtures
  3. customobtained
  4. filtrationthe solid is filtered off
  5. washrinsed with diethylene glycol dimethyl ether
  6. washthe filtrate and wash solutions
  7. customThe majority of the solvent is removed
  8. addition300 ml water are added to the concentrated solution (approx. 50 ml)
  9. customthe solid obtained
  10. filtrationis filtered off
  11. washwashed once with water
  12. customdried under a high vacuum

出典と根拠

ORDレコード
ord-9515b47fdaa94e3b925ae0dc67765780
出典データセット
uspto-grants-2014_02
特許番号
US08653111B2

反応ノート

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