Methanol → HCID 68700047, compound
Reaction equation
Cl[N:2]1[CH:7](Cl)[CH2:6][NH:5][CH2:4][CH2:3]1.[CH3:9][O-:10].[Na+].[CH3:12][OH:13]>>[CH3:9][O:10][N:2]1[CH:7]([O:13][CH3:12])[CH2:6][NH:5][CH2:4][CH2:3]1Participants
4
Procedure
A mixture of 1,6-dichloropiperazine U (3.9 g; 26 mmol) and freshly prepared sodium methoxide (62 mmol) in anhydrous methanol (50 ml) was refluxed overnight and the solvent was removed under reduced pressure. The residue was diluted to 100 ml with CH2Cl2 and the solution washed with water, brine and dried over anhydrous MgSO4 and filtered off. The filtrate was evaporated under reduced pressure to give pure 1,6-dimethoxypiperazine V (3.6 g; 98%) as a colourless crystals. 1HNMR (CDCl3) 3.94 (s, 6H); 7.76 (s, 2H).
Workup
- temperaturewas refluxed overnight
- customthe solvent was removed under reduced pressure
- additionThe residue was diluted to 100 ml with CH2Cl2
- washthe solution washed with water, brine
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered off
- customThe filtrate was evaporated under reduced pressure
Sources & evidence
- ORD record
- ord-7eb529090e324cd6a8b2ffec20b3df45
- Source dataset
- uspto-grants-2013_06
- Patent number
- US08466163B2
Reaction notes
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