Water → HCID 57599729, compound
Reaction equation
[NH2:1][C:2]1[C:9]([O:10][CH3:11])=[C:8]([O:12][CH2:13][O:14][CH3:15])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=S.O.[CH2:31](N)[CH2:32][NH2:33]>>[NH:5]1[CH2:31][CH2:32][N:33]=[C:4]1[C:3]1[C:2]([NH2:1])=[C:9]([O:10][CH3:11])[C:8]([O:12][CH2:13][O:14][CH3:15])=[CH:7][CH:6]=1Participants
5
Procedure
A solution of 2-amino-3-methoxy-4-(methoxymethoxy)benzonitrile 475 mg (2.28 mmol) and phosphorus pentasulfide 25.4 mg (0.11 mmol) in ethylenediamine 2.75 g was stirred at 120° C. for overnight. The reaction mixture was cooled to room temperature and poured into water. The precipitate was collected and washed with water to give the title compound 293 mg as white solid. Yield 51.1%.
Workup
- customThe precipitate was collected
- washwashed with water
Sources & evidence
- ORD record
- ord-e5e38a8a6fc44a56ac82c67cfa169304
- Source dataset
- uspto-grants-2009_03
- Patent number
- US07511041B2
Reaction notes
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