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N,N-Diethylethylenediamine → HCID 70549843, compound

HRID 1413150
Notes
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Reaction equation

HRID 1413150 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]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

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-3c6957352f854d9ea6f5a7c86e33c7c3
Source dataset
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04248885

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes