Bromine → HCID 178517592, 화합물

HRID 517971노트

반응식

HRID 517971 반응식
[OH:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[Br:12]Br>CO>[Br:12][C:5]1[CH:6]=[C:7]([C:8]([F:9])([F:11])[F:10])[C:2]([OH:1])=[N:3][CH:4]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 36784112(1H)-Pyridinone, 3-(trifluoromethyl)-

생성물 1

HCID 178517592HCID 178517592, 화합물수율 94.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 2-hydroxy-3-(trifluoromethyl)pyridine (10.0 g) and bromine (3.08 ml, 9.60 g) in methanol (50 ml) was stirred at 20° C. for 22 h. The solution was concentrated and the residue partitioned between ethyl acetate (400 ml) and water (100 ml). The layers were separated and the organic layer was washed with 5% Na2S2O3aq. (100 ml) and brine (100 ml), dried over sodium sulphate, filtered and concentrated. Purified by Biotage SNAP cartridge KP-Sil column twice (100 g, heptane:ethyl acetate=1:0, 3:1 to 2:1) to give 13.69 g light yellow solid as 5-bromo-2-hydroxy-3-(trifluoromethyl)pyridine (95%).

후처리

  1. concentrationThe solution was concentrated
  2. customthe residue partitioned between ethyl acetate (400 ml) and water (100 ml)
  3. customThe layers were separated
  4. washthe organic layer was washed with 5% Na2S2O3aq
  5. dry with material(100 ml) and brine (100 ml), dried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customPurified by Biotage SNAP cartridge KP-Sil column twice (100 g, heptane:ethyl acetate=1:0, 3:1 to 2:1)

출처 및 근거

ORD 기록
ord-a9b9b295723d4dd89022c3f180cfbf97
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115126B2

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