Diethylamine → HCID 23332913, compound

HRID 224395Notes

Reaction equation

HRID 224395 reaction equation
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[Cl:6][C:7]([Cl:27])([Cl:26])[CH:8]1[O:13][CH:12]([C:14]([Cl:17])([Cl:16])[Cl:15])[C:11]2[CH:18]=[C:19]([S:22](Cl)(=[O:24])=[O:23])[CH:20]=[CH:21][C:10]=2[O:9]1>C(O)C>[CH2:1]([N:3]([CH2:4][CH3:5])[S:22]([C:19]1[CH:20]=[CH:21][C:10]2[O:9][CH:8]([C:7]([Cl:6])([Cl:26])[Cl:27])[O:13][CH:12]([C:14]([Cl:17])([Cl:15])[Cl:16])[C:11]=2[CH:18]=1)(=[O:24])=[O:23])[CH3:2]

Participants

4

Reactant 2

HCID 8021DiethylamineHCID 233329662,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-sulfonyl chloride

Product 1

HCID 23332913HCID 23332913, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Diethylamine (0.8 g.) was added dropwise to a stirred suspension of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-sulphonyl chloride (4.7 g.) in absolute ethanol (20 ml.), the mixture was maintained under gentle reflux for 2 hours, and the resulting solution was allowed to cool slowly to give a crystalline product, which was recrystallised from aqueous methanol to give 6-diethylsulphamoyl-2,4-bis(trichloromethyl)benzo[1,3]dioxin, m.p. 125°-126° C.

Workup

  1. temperaturethe mixture was maintained
  2. temperatureunder gentle reflux for 2 hours
  3. temperatureto cool slowly
  4. customto give a crystalline product, which
  5. customwas recrystallised from aqueous methanol

Sources & evidence

ORD record
ord-9135a77f0285445f92e484d3083d62fa
Source dataset
uspto-grants-1980_11
Patent number
US04232032

Reaction notes

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