Ammonia → 6-(2-Hydroxyphenyl)-3(2H)-pyridazinone

HRID 370753노트

반응식

HRID 370753 반응식
O[CH:2]([CH2:6][C:7](=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[OH:14])[C:3](O)=[O:4].Cl.[NH2:17][NH2:18].N>O.C(O)(=O)C.C(N(CC)CC)C>[OH:14][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[C:7]1[CH:6]=[CH:2][C:3](=[O:4])[NH:17][N:18]=1

참가 물질

8

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 9321HydrazineHCID 13778436HCID 13778436, 화합물

생성물 1

HCID 30173466-(2-Hydroxyphenyl)-3(2H)-pyridazinone수율 78.3%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 8471Triethylamine용매

실험 절차

To a stirred suspension of 2-hydroxy-4-oxo-4-(2-hydroxyphenyl)butyric acid (0.025M) in water (20 ml) was added triethylamine (3.3 ml), taking the pH to 9.5, followed by concentrated hydrochloric acid (2.5 ml) to take the pH to 4. Hydrazine (0.05M) was added slowly with the concurrent addition of sufficient glacial acetic acid to maintain a pH of 7.0. Steam heating was applied for 2 hours and during this time the pH of 7.0 was maintained by the addition of ammonia as necessary. The reaction mixture was allowed to cool to room temperature. The solid was filtered off, washed with water, 2-propanol and dried to afford 6-(2-hydroxyphenyl)-3(2H)-pyridazinone (78.3%).

후처리

  1. temperatureto maintain a pH of 7.0
  2. temperatureSteam heating
  3. filtrationThe solid was filtered off
  4. washwashed with water, 2-propanol
  5. customdried

출처 및 근거

ORD 기록
ord-77b26cc6ff1148b685509d4ad536726f
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528371

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