Phenol → HCID 21217669, compound
Reaction equation
[Na].Cl[C:3]1[N:4]=[N:5][C:6]([S:9][CH2:10][CH:11]=[CH2:12])=[CH:7][CH:8]=1.[C:13]1([OH:19])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>>[O:19]([C:3]1[N:4]=[N:5][C:6]([S:9][CH2:10][CH:11]=[CH2:12])=[CH:7][CH:8]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1Participants
4
Conditions
- Temperature
- 160 °C
Procedure
0.11 g(0.005 mol) of metallic sodium was dissolved in 30 g of dry phenol. To the resulting solution was added 0.93 g(0.005 mol) of 3-chloro-6-allylthiopyridazine and then the reaction solution was stirred for 3 hours at 160±5° C. After the reaction was allowed to stop, the reaction solution was cooled and adjusted to alkaline (pH 14) with 2N--NaOH, thereby precipitating the crystals. The precipitated crystal was extracted with diethyl ether and then treated according to the same manner as Example 1 to obtain the title compound as a crystal.
Workup
- temperaturethe reaction solution was cooled
- customNaOH, thereby precipitating the crystals
- extractionThe precipitated crystal was extracted with diethyl ether
- additiontreated
Sources & evidence
- ORD record
- ord-2571025325ce4872a997c0b9cbe25cda
- Source dataset
- uspto-grants-1999_08
- Patent number
- US05942511
Reaction notes
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