Potassium Carbonate → HCID 65369304、化合物

HRID 1409524ノート

反応式

HRID 1409524 の反応式
[Br:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:15]([O:17][CH2:18]Cl)[CH3:16]>CC(C)=O>[Br:1][C:2]1[C:7]([O:8][CH2:18][O:17][CH2:15][CH3:16])=[CH:6][CH:5]=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 18523Chloromethyl ethyl etherHCID 230702-Bromo-3-pyridinol

生成物 1

HCID 65369304HCID 65369304、化合物収率 88.9%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a RBF was added 2-bromo-3-pyridinol (6.0 g, 34.5 mmol) and potassium carbonate (11.91 g, 86 mmol) in Acetone (50 mL). The suspension was stirred at ambient temperature for 30 min and then treated with the drop-wise addition of chloromethyl ethyl ether (3.34 mL, 36.7 mmol) via addition funnel. The mixture was stirred at ambient temperature overnight. The mixture was filtered and the filtrate partitioned between EtOAc and water. The combined organic layers were washed with water, saturated solution of sodium bicarbonate and brine, then dried over Mg2SO4 to afford 7.12 g of desired product as a clear oil which was used without further purification.

後処理

  1. stirringThe mixture was stirred at ambient temperature overnight
  2. filtrationThe mixture was filtered
  3. customthe filtrate partitioned between EtOAc and water
  4. washThe combined organic layers were washed with water, saturated solution of sodium bicarbonate and brine
  5. dry with materialdried over Mg2SO4

出典と根拠

ORDレコード
ord-78edc630e1644e4796a4b93a67eaea36
出典データセット
uspto-grants-2014_12
特許番号
US08921363B2

反応ノート

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