Thiourea → HCID 20160623, compound

HRID 247394Notes

Reaction equation

HRID 247394 reaction equation
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH2:15][CH2:16][CH3:17])=[C:10]([O:18][CH3:19])[CH:9]=2)=[CH:6][CH:7]=1.NC(N)=[S:22]>COCCO.O>[CH3:19][O:18][C:10]1[CH:9]=[C:8]([C:5]2[CH:6]=[CH:7][C:2](=[S:22])[NH:3][N:4]=2)[CH:13]=[CH:12][C:11]=1[O:14][CH2:15][CH2:16][CH3:17]

Participants

5

Reactant 2

HCID 2723790ThioureaHCID 193854943-Chloro-6-(3-methoxy-4-propoxyphenyl)pyridazine

Product 1

HCID 20160623HCID 20160623, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 80192-MethoxyethanolSolvent

Procedure

T13.9 g of 3-chloro-6-(3-methoxy-4-n-propoxyphenyl)pyridazine are boiled under reflux with 5.5 g of thiourea in 50 ml of ethylene glycol monomethyl ether for 8 hours. After cooling, the mixture is diluted with 250 ml of water and extracted three times with chloroform. The chloroform extracts are dried over sodium sulfate and evaporated. The residue is crystallized from ethanol/ethyl acetate. 4.8 g (34.6% of theory) of the title compound of m.p. 174°-17620 are obtained.

Workup

  1. temperatureAfter cooling
  2. extractionextracted three times with chloroform
  3. dry with materialThe chloroform extracts are dried over sodium sulfate
  4. customevaporated
  5. customThe residue is crystallized from ethanol/ethyl acetate

Sources & evidence

ORD record
ord-6abbad248c5a42f7be0c2121b9e67689
Source dataset
uspto-grants-1987_11
Patent number
US04707481

Reaction notes

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