Acetic Acid → HCID 178474109, 화합물

HRID 1112321노트

반응식

HRID 1112321 반응식
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Br:11])[N:6]=1)(=[O:3])[CH3:2].C(O)(=[O:14])C.C(OO)(=O)C>O>[C:1]([NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Br:11])[N+:6]=1[O-:14])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 6585Peracetic AcidHCID 10353221N-(6-bromopyridin-2-yl)acetamide

생성물 1

HCID 178474109HCID 178474109, 화합물수율 83%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

23.4 gms (0.109 mole) of 2-acetamido-6-bromopyridine was dissolved in 200 ml. of glacial acetic acid containing 27.6 ml (0.218 mole) of 7.9M peracetic acid and the solution was heated at 70° C. for 2 hours and at 55° C. for 19 hours. The reaction mixture was diluted with 1600 ml water and the solution was then concentrated in vacuo to 550 ml. 8.6% of unreacted-2-acetamido-6-bromopyridine was removed by filtration. The solvent was evaporated from the filtrate giving an 83% yield of impure 2-acetamido-6-bromopyridine-1-oxide which was purified by treatment with activated charcoal to remove the yellow impurity and subsequently recrystallized from 2-propanol. A second recrystallization from 2-propanol gave fine white needles, m.p=180.0°-180.5° C.

후처리

  1. concentrationthe solution was then concentrated in vacuo to 550 ml
  2. custom8.6% of unreacted-2-acetamido-6-bromopyridine was removed by filtration
  3. customThe solvent was evaporated from the filtrate

출처 및 근거

ORD 기록
ord-8753e94e030e410e8ac0179627b8a51f
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04122085

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