Potassium Carbonate → HCID 18770388, compound

HRID 1279459Notes

Reaction equation

HRID 1279459 reaction equation
C(=O)([O-])[O-].[K+].[K+].Cl.Cl.Cl.Cl.[N:11]1([CH2:18][CH2:19][CH2:20][N:21]2[CH2:27][CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH2:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1>O>[N:11]1([CH2:18][CH2:19][CH2:20][N:21]2[CH2:27][CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH2:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 69492385HCID 69492385, compound

Product 1

HCID 18770388HCID 18770388, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Potassium carbonate (0.50 g; 3.6 mmol) was added to a solution in water (1 ml) of 1,1′-trimethylenedi(hexahydro-1,4-diazepine) tetrahydrochloride (540 mg; 1.4 mmol) synthesized in accordance with the same process as in Referential Example 1. The mixture was stirred at room temperature for 15 minutes and concentrated under reduced pressure. A process of adding ethanol (10 ml) to the residue and concentrating the mixture under reduced pressure was conducted twice. The resultant concentrated residue was purified by column chromatography on silica gel, thereby obtaining 323 mg (yield: 96%) of 1,1′-trimethylenedi(hexahydro-1,4-diazepine) as a colorless oil.

Workup

  1. customsynthesized in accordance with the same process as in Referential Example 1
  2. concentrationconcentrated under reduced pressure
  3. concentrationA process of adding ethanol (10 ml) to the residue and concentrating the mixture under reduced pressure
  4. customThe resultant concentrated residue was purified by column chromatography on silica gel

Sources & evidence

ORD record
ord-4c7a56692a4e40208875f4e7d7748bcc
Source dataset
uspto-grants-2002_09
Patent number
US06448242B1

Reaction notes

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