Hydroxylamine → 51519-20-1
Reaction equation
C[N:2](C)[CH:3]=[N:4][C:5]1[CH:10]=[N:9][CH:8]=[CH:7][N:6]=1.N[OH:13]>O1CCCC1>[OH:13][NH:2][CH:3]=[N:4][C:5]1[CH:10]=[N:9][CH:8]=[CH:7][N:6]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
A solution of N,N-dimethyl-N′-pyrazin-2-ylimidoformamide (189 g) from Step A in tetrahydrofuran (400 mL) was treated drop wise with 50% aqueous solution of hydroxylamine (245.7 mL) at 0° C., then warmed up to 80° C. for 2.5 h. Tetrahydrofuran was removed by rotoevaporation and the resulting aqueous mixture kept cold in a refrigerator. The resulting solid was filtered and rinsed with cold diethyl ether to yield the desired product.
Workup
- customTetrahydrofuran was removed by rotoevaporation
- filtrationThe resulting solid was filtered
- washrinsed with cold diethyl ether
Sources & evidence
- ORD record
- ord-354e37c2d3d34199aa47b4bed8435fd3
- Source dataset
- uspto-grants-2009_01
- Patent number
- US07482336B2
Reaction notes
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