Hydrochloric Acid → HCID 20456935, compound
Reaction equation
[CH3:1][S:2]([N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)(=[O:4])=[O:3].Cl.[O-]C#[N:14].[K+].Cl[O-].[Na+].Cl[O-]>O>[NH2:14][CH2:1][S:2]([N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)(=[O:4])=[O:3]Participants
Procedure
10 g of methanesulfonyl-piperazine are dissolved in 50 ml of water; after adding 6.2 ml of concentrated hydrochloric acid thereto, a solution of 5.4 g of potassium cyanate in 20 ml of water is added dropwise, and the thus-obtained mixture is stirred for 4 hours at room temperature. The precipitate which separates out is filtered off and dried. Yield: 11 g; melting point: 254° C. 10 g of the dried precipitate and 4 g of sodium hydroxide solution in 80 ml of water are cooled to 0° C., and 0.052 mol of sodium hypochlorite, which has been pre-cooled to 0° C., is added. The mixture is then stirred at room temperature until no further hypochlorite is detectable. The aqueous solution of 1-aminomethanesulfonylpiperazine, which is obtained in this way, is directly useful in the further reaction.
Workup
- filtrationThe precipitate which separates out is filtered off
- customdried
- temperature10 g of the dried precipitate and 4 g of sodium hydroxide solution in 80 ml of water are cooled to 0° C.
- additionis added
Sources & evidence
- ORD record
- ord-38b3ed906efd4b9096f6259f23ba5b9e
- Source dataset
- uspto-grants-1982_06
- Patent number
- US04332801
Reaction notes
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