Sodium Hydroxide → HCID 136351291, compound

HRID 1599700Notes

Reaction equation

HRID 1599700 reaction equation
[OH-].[Na+].Cl.Cl.[NH:5]=[C:6]([NH:12][C:13](=[O:22])[O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)N1C=CC=N1.Cl.Cl.[NH2:25][CH2:26][CH:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1>O>[NH2:25][CH2:26][CH:27]1[CH2:32][CH2:31][N:30]([N:5]=[CH:6][NH:12][C:13](=[O:22])[O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:29][CH2:28]1

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 19079009HCID 19079009, compoundHCID 178478782HCID 178478782, compound

Product 1

HCID 136351291HCID 136351291, compoundYield 95%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Sodium hydroxide (4.45 g, 111.25 mmole) was dissolved in 150 mL of deionized water. The mixture of [imino(1H-pyrazol-1-yl)methyl]carbamic acid, phenylmethyl ester, dihydrochloride salt and 4-aminomethyl piperidine, dihydrochloride salt (prepared above, 16.18 g, 44.54 mmole) was added (pH of the cloudy solution was 13) and the mixture was extracted with dichloromethane (1×200 mL and 2×100 mL). The organic layers were combined and washed with brine (1×200 mL), dried (MgSO4), filtered and concentrated in vacuo to provide the title compound as a white foam (12.29 g, 95%).

Workup

  1. additionwas added (pH of the cloudy solution
  2. extractionwas extracted with dichloromethane (1×200 mL and 2×100 mL)
  3. washwashed with brine (1×200 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-a80ce5efb09f402ea72119c6c916e17b
Source dataset
uspto-grants-1998_04
Patent number
US05741792

Reaction notes

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