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

HRID 370753ノート

反応式

HRID 370753 の反応式
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

参加物

8

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 9321HydrazineHCID 13778436HCID 13778436、化合物

生成物 1

HCID 30173466-(2-Hydroxyphenyl)-3(2H)-pyridazinone収率 78.3%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 8471Triethylamine溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-77b26cc6ff1148b685509d4ad536726f
出典データセット
uspto-grants-1985_07
特許番号
US04528371

反応ノート

読み込み中…