Acetyl bromide → HCID 86703139、化合物

HRID 2204333ノート

反応式

HRID 2204333 の反応式
[CH3:1][O:2][C:3]1[C:4]([N+]([O-])=O)=[CH:5][C:6]([CH3:10])=[N+:7]([O-:9])[CH:8]=1.C([Br:17])(=O)C>C(O)(=O)C>[Br:17][C:4]1[C:3]([O:2][CH3:1])=[CH:8][N+:7]([O-:9])=[C:6]([CH3:10])[CH:5]=1

参加物

4

反応物 2

HCID 10482Acetyl bromideHCID 151634575-Methoxy-2-methyl-4-nitropyridine 1-oxide

生成物 1

HCID 86703139HCID 86703139、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

5-Methoxy-2-methyl-4-nitro-pyridine-1-oxide (Step AL5) (1.9 g, 10.3 mmol) and acetyl bromide (22.9 mL, 310 mmol) was added to acetic acid (40 mL) and the reaction was stirred at 80° C. for 1 h. The mixture was concentrated (1/3) and a solution of NaOH was added. The resulting mixture was extracted with EtOAc, washed with brine, dried (Na2SO4), filtered and concentrated. The product was crystallised (EtOAc/TBME). ESI-MS: tR=0.54 min, [M+H]+ 218.1/220.1 (LC-MS 1).

後処理

  1. concentrationThe mixture was concentrated (1/3)
  2. additiona solution of NaOH was added
  3. extractionThe resulting mixture was extracted with EtOAc
  4. washwashed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe product was crystallised (EtOAc/TBME)

出典と根拠

ORDレコード
ord-f96c31e4869147be9d38b9522a6a9647
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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