Bromine → HCID 178517592、化合物

HRID 517971ノート

反応式

HRID 517971 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 178517592HCID 178517592、化合物収率 94.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-a9b9b295723d4dd89022c3f180cfbf97
出典データセット
uspto-grants-2015_08
特許番号
US09115126B2

反応ノート

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