Phosphorus tribromide → 4-Bromo-5-methoxy-2-methylpyridine

HRID 2204332ノート

反応式

HRID 2204332 の反応式
[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N+:5]([O-])=[C:4]([CH3:11])[CH:3]=1.P(Br)(Br)Br>C(Cl)(Cl)Cl.C(Cl)Cl>[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]=[C:4]([CH3:11])[CH:3]=1

参加物

5

反応物 2

HCID 24614Phosphorus tribromideHCID 86703139HCID 86703139、化合物

生成物 1

HCID 735548294-Bromo-5-methoxy-2-methylpyridine

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-bromo-5-methoxy-2-methyl-pyridine 1-oxide (Step AL4) (150 mg, 0.7 mmol) in CHCl3 (2 mL) at 10° C. was added dropwise PBr3 (78 μL, 0.826 mmol). The mixture was stirred at rt for 4 h, then at 50° C. for 1 h. The reaction mixture was dissolved in CH2Cl2 and extracted with a saturated aqueous solution of NaHCO3, washed with brine, dried (Na2SO4), filtered and concentrated. The product was crystallised (CH2Cl2/TBME). ESI-MS: tR=0.69 min, [M+H]+ 202.0/204.0 (LC-MS 1).

後処理

  1. waitat 50° C. for 1 h
  2. extractionextracted with a saturated aqueous solution of NaHCO3
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe product was crystallised (CH2Cl2/TBME)

出典と根拠

ORDレコード
ord-20be6cdbf5344d469023a46bad09fda7
出典データセット
uspto-grants-2016_06
特許番号
US09365576B2

反応ノート

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