Hydrazine hydrate (1:1) → 4-(3-Chlorophenyl)pyridazine-3,6-diol

HRID 2239888노트

반응식

HRID 2239888 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:9](=O)[O:10][C:11](=[O:13])[CH:12]=2)[CH:5]=[CH:6][CH:7]=1.O.[NH2:16][NH2:17]>O.C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:12]=[C:11]([OH:13])[N:17]=[N:16][C:9]=2[OH:10])[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 86618521HCID 86618521, 화합물

생성물 1

HCID 1785155844-(3-Chlorophenyl)pyridazine-3,6-diol

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

To a 25 mL flask was added 3-(3-chlorophenyl)furan-2,5-dione (1.7 g, 8.15 mmol) from (1a) and hydrazine hydrate (0.476 mL, 9.78 mmol) in water (6 mL) and acetic acid (4 mL). The resulting mixture was refluxed for 18 hours. The solution was cooled and placed in the refrigerator for 1 hour. The resulting precipitate was filtered and dried, then purified by flash chromatography eluting with 5% methanol/dichloromethane to give 4-(3-chlorophenyl)pyridazine-3,6-diol.

후처리

  1. temperatureThe resulting mixture was refluxed for 18 hours
  2. temperatureThe solution was cooled
  3. filtrationThe resulting precipitate was filtered
  4. customdried
  5. custompurified by flash chromatography
  6. washeluting with 5% methanol/dichloromethane

출처 및 근거

ORD 기록
ord-a2a103fb8fb34b94a6d33ca5cde93a59
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723336B2

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