Hydrochloric Acid → HCID 178515445、化合物

HRID 594045ノート

反応式

HRID 594045 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4](Cl)[CH:3]=1.Cl.[O:11]1CCOCC1>[OH-].[Na+]>[Br:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([OH:11])[CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 202807664-Bromo-2,6-dichloropyridine

生成物 1

HCID 178515445HCID 178515445、化合物収率 76%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 4-bromo-2,6-dichloropyridine (1.0 equiv.) in dioxane and aqueous sodium hydroxide (15% by weight solution, 1:1 ratio, 0.55 M) was heated in the microwave for 30 min at 150° C. The solution was cooled to room temperature and neutralized with concentrated HCl (pH=˜6) and extracted with ethyl acetate three times. The organic phase was dried with sodium sulfate, filtered and concentrated. The crude material was dried under vacuo to give 4-bromo-6-chloropyridin-2-ol as an off-white solid in 76% yield. LCMS (m/z) (M+H)=207.9/209.9, Rt=0.60 min.

後処理

  1. extractionextracted with ethyl acetate three times
  2. dry with materialThe organic phase was dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. dry with materialThe crude material was dried under vacuo

出典と根拠

ORDレコード
ord-222f807389dc42f79e1badf4cf1dff3f
出典データセット
uspto-grants-2016_01
特許番号
US09242969B2

反応ノート

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