N,N-Diethylethylenediamine → HCID 70549843, compound

HRID 2052627Notes

Reaction equation

HRID 2052627 reaction equation
[CH2:1]([N:3]([CH2:6][CH2:7][NH2:8])[CH2:4][CH3:5])[CH3:2].[O:9]1[C:14]2[CH:15]=[CH:16][CH:17]=[C:18]([C:19]([Cl:21])=[O:20])[C:13]=2[O:12][CH2:11][CH2:10]1>CC(C)=O>[ClH:21].[CH2:1]([N:3]([CH2:6][CH2:7][NH:8][C:19]([C:18]1[C:13]2[O:12][CH2:11][CH2:10][O:9][C:14]=2[CH:15]=[CH:16][CH:17]=1)=[O:20])[CH2:4][CH3:5])[CH3:2]

Participants

4

Reactant 2

HCID 60993N,N-DiethylethylenediamineHCID 27950312,3-Dihydro-1,4-benzodioxine-5-carbonyl chloride

Product 1

HCID 70549843HCID 70549843, compoundYield 64.2%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Conditions

Temperature
0 °C

Procedure

21 g of diethylaminoethylamine and 85 ml of acetone were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was cooled to 0° C. and then 36 g of 1,4-benzodioxane-5-carbonyl chloride were added. The crystals formed at ambient temperature were dried off, washed with acetone, dried and purified by recrystallization from isopropyl alcohol. 36.5 g of N-(diethylaminoethyl)-1,4-benzodioxane-5-carboxamide hydrochloride were obtained (M.P.: 120° C.; yield: 64%).

Workup

  1. customprovided with an agitator
  2. customThe crystals formed at ambient temperature
  3. customwere dried off
  4. washwashed with acetone
  5. customdried
  6. custompurified by recrystallization from isopropyl alcohol

Sources & evidence

ORD record
ord-60d094da16fd453898d6a544c6f22341
Source dataset
uspto-grants-1980_01
Patent number
US04186135

Reaction notes

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