Hydrochloric Acid → HCID 178515445, 화합물

HRID 594045노트

반응식

HRID 594045 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178515445HCID 178515445, 화합물수율 76%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-222f807389dc42f79e1badf4cf1dff3f
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242969B2

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