Hydrazine Sulfate → 4-Bromopyridazine-3,6-diol

HRID 15168

반응식

HRID 15168 반응식
S(O)(O)(=O)=O.[NH2:6][NH2:7].[Br:8][C:9]1[C:10](O[C:13](=[O:15])[CH:14]=1)=[O:11]>O>[Br:8][C:9]1[C:10](=[O:11])[NH:6][NH:7][C:13](=[O:15])[CH:14]=1

참가 물질

4

반응물 2

HCID 24842Hydrazine Sulfate2회HCID 800273-Bromo-2,5-furandione2회

생성물 1

HCID 2549424-Bromopyridazine-3,6-diol수율 151%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Hydrazine sulphate salt (51 g) was suspended in water (250 ml), heated to reflux and bromomaleic anhydride (90.38 g) was added dropwise. The mixture was heated at reflux for 4 hours then cooled to room temperature. The reaction was repeated with 29 g hydrazine sulphate, 53 g bromomaleic anhydride and 130 ml water. The precipitates were collected by filtration, washed with water and acetone and dried as a combined batch in vacuo to afford 4-bromo-1,2-dihydro-3,6-pyridazinedione as a white solid (113 g).

후처리

  1. temperatureheated
  2. temperatureto reflux
  3. temperatureThe mixture was heated
  4. temperatureat reflux for 4 hours
  5. filtrationThe precipitates were collected by filtration
  6. washwashed with water and acetone
  7. customdried as a combined batch in vacuo

출처 및 근거

ORD 기록
ord-d45f37f166944474839658fa69d9d642
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732460B2

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