Acetyl bromide → HCID 86703139, 화합물

HRID 2204333노트

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HRID 2204333 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 86703139HCID 86703139, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
80 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-f96c31e4869147be9d38b9522a6a9647
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365576B2

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