Diethylamine → HCID 23332927, compound

HRID 224391Notes

Reaction equation

HRID 224391 reaction equation
[Cl:1][C:2]([Cl:21])([Cl:20])[CH:3]1[O:8][CH:7]([C:9](Cl)([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17](Cl)=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.[CH2:22]([NH:24][CH2:25][CH3:26])[CH3:23]>>[Cl:10][C:9]([Cl:11])=[C:7]1[C:6]2[CH:13]=[C:14]([C:17]([N:24]([CH2:25][CH3:26])[CH2:22][CH3:23])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4][CH:3]([C:2]([Cl:20])([Cl:21])[Cl:1])[O:8]1

Participants

3

Reactant 2

HCID 8021DiethylamineHCID 233329602,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-carbonyl chloride

Product 1

HCID 23332927HCID 23332927, compound

Procedure

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carbonyl chloride (2 g.) and diethylamine (25 ml.) was heated under reflux for 2 hrs., cooled, and filtered to remove diethylamine hydrochloride. The filtrate was evaporated to dryness under reduced pressure, and the residue was crystallised from ethanol to give 4-dichloromethylene-N,N-diethyl-2-trichloromethylbenzo[1,3]dioxin-6-carboxamide, m.p. 123°-124° C.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hrs
  3. temperature, cooled
  4. filtrationfiltered
  5. customto remove diethylamine hydrochloride
  6. customThe filtrate was evaporated to dryness under reduced pressure
  7. customthe residue was crystallised from ethanol

Sources & evidence

ORD record
ord-79420fbaf6684c2cb28d487ece978294
Source dataset
uspto-grants-1980_11
Patent number
US04232032

Reaction notes

Loading…