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Dichloromethane → (4-Bromo-5-methylpyridin-2-yl)methanol

HRID 2080477
ノート
印刷プレビュー

反応式

HRID 2080477 の反応式
FC(F)(F)C(O[C:6](=[O:11])[C:7](F)(F)F)=O.ClCCl.[Br:17][C:18]1[C:23]([CH3:24])=[CH:22][N+:21]([O-])=C(C)[CH:19]=1>CCCCCC>[Br:17][C:18]1[C:23]([CH3:24])=[CH:22][N:21]=[C:7]([CH2:6][OH:11])[CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 9845Trifluoroacetic anhydrideHCID 544438594-Bromo-2,5-dimethylpyridine 1-oxide

生成物 1

HCID 23114663(4-Bromo-5-methylpyridin-2-yl)methanol収率 83.3%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

Under an argon atmosphere, trifluoroacetic anhydride (20.6 ml, 0.146 mol) was added to a dichloromethane solution (100 ml) solution of 4-bromo-2,5-dimethylpyridine 1-oxide (9.8 g, 48.5 mmol) under ice cooling. The resulting mixture was stirred for 20 minutes and then, stirred at room temperature for 7.5 hours. The reaction mixture was concentrated under reduced pressure. To a dichloromethane solution (50 ml) of the residue was added a saturated aqueous solution (100 ml) of sodium bicarbonate. The resulting mixture was stirred for 14 hours. The reaction mixture was extracted with dichloromethane. The extract was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate (=1:1) eluate was concentrated under reduced pressure to give the title compound (8.17 g, 40.4 mmol, 83%) as a yellow powder.

後処理

  1. stirringstirred at room temperature for 7.5 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionTo a dichloromethane solution (50 ml) of the residue was added a saturated aqueous solution (100 ml) of sodium bicarbonate
  4. stirringThe resulting mixture was stirred for 14 hours
  5. extractionThe reaction mixture was extracted with dichloromethane
  6. dry with materialThe extract was dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue thus obtained
  9. concentrationethyl acetate (=1:1) eluate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-406bae1fc46848bb8fac4917346b95d2
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932271B2

反応ノート

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