Potassium Carbonate → HCID 18427419, compound

HRID 1279458Notes

Reaction equation

HRID 1279458 reaction equation
C(=O)([O-])[O-].[K+].[K+].Cl.Cl.Cl.Cl.[CH2:11]([N:20]1[CH2:26][CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)[CH2:12][N:13]1[CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>O>[CH2:11]([N:20]1[CH2:26][CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)[CH2:12][N:13]1[CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 18427418HCID 18427418, compound

Product 1

HCID 18427419HCID 18427419, compoundYield 104.3%

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′-ethylenedi(hexahydro-1,4-diazepine)tetrahydrochloride (385 mg; 1.0 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 performed twice. The resultant concentrated residue was purified by column chromatography on silica gel, thereby obtaining 236 mg (yield: 69%) of 1,1′-ethylenedi(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-d473261b83144487a52c18ff6a228de1
Source dataset
uspto-grants-2002_09
Patent number
US06448242B1

Reaction notes

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