Sodium Methoxide → HCID 14220967、化合物

HRID 568385ノート

反応式

HRID 568385 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([CH3:12])[CH:11]=1)[N:8]=[C:7](Cl)[CH:6]=[CH:5]2.[CH3:14][O-:15].[Na+]>CO>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([CH3:12])[CH:11]=1)[N:8]=[C:7]([O:15][CH3:14])[CH:6]=[CH:5]2

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 142210366-Bromo-2-chloro-8-methylquinoline

生成物 1

HCID 14220967HCID 14220967、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 6-bromo-2-chloro-8-methylquinoline (10.7 g) in methanol (80 cm3) was heated under reflux with a solution of sodium methoxide [made from sodium (2.76 g) in methanol (50 cm3)] for 24 hours. The cooled solution was then evaporated in vacuo and the residue was partitioned between chloroform (100 cm3) and water (50 cm3). The aqueous phase was further extracted with chloroform (2×50 cm3) and the combined and dried (MgSO4) organic phases were evaporated in vacuo to give a solid which was recrystallised from ethyl acetate:hexane, 1:9, to afford 6-bromo-2-methoxy-8-methylquinoline, m.p. 89°-91° (8.3 g).

後処理

  1. customThe cooled solution was then evaporated in vacuo
  2. customthe residue was partitioned between chloroform (100 cm3) and water (50 cm3)
  3. extractionThe aqueous phase was further extracted with chloroform (2×50 cm3)
  4. dry with materialdried (MgSO4) organic phases
  5. customwere evaporated in vacuo
  6. customto give a solid which
  7. customwas recrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-f595c9dd513341c196ba5a271675b279
出典データセット
uspto-grants-1988_03
特許番号
US04728653

反応ノート

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