Dimethylcarbamoyl Chloride → HCID 86652108, compound

HRID 1912214Notes

Reaction equation

HRID 1912214 reaction equation
CN(C)C(Cl)=[O:4].[CH2:7]([N:9]([CH2:12][CH3:13])[CH2:10][CH3:11])C.[NH2:14][CH2:15][CH2:16][CH2:17][OH:18]>O1CCOCC1>[OH:18][CH2:17][CH2:16][CH2:15][NH:14][C:7](=[O:4])[N:9]([CH2:12][CH3:13])[CH2:10][CH3:11]

Participants

5

Reactant 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 90863-Amino-1-propanol

Product 1

HCID 86652108HCID 86652108, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
90 °C

Procedure

15.0 g (139.5 mmol) of N,N-dimethylcarbamoyl chloride and 80 mL dioxane were added to a 250 mL two-necked flask with a reflux condenser. Then 13.66 g (135 mmol) triethylamine and 10.44 g (139 mmol) of 3-amino-1-propanol were added. After exothermic evolution of heat subsided, the mixture was stirred for 1 h at 60° C. and for 3 h at 90° C., where a light brown suspension slowly formed. After the suspension had been cooled down to 50° C., the solid was filtered out.

Workup

  1. temperatureAfter exothermic evolution of heat
  2. customwhere a light brown suspension slowly formed
  3. temperatureAfter the suspension had been cooled down to 50° C.
  4. filtrationthe solid was filtered out

Sources & evidence

ORD record
ord-e2f40592fa69481295c14543ddb8fe4f
Source dataset
uspto-grants-2013_12
Patent number
US08608899B2

Reaction notes

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