Diethylamine → HCID 67745068, compound

HRID 1078311Notes

Reaction equation

HRID 1078311 reaction equation
Cl[C:2]1[C:3]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:4]=2[S:5](=[O:9])(=[O:8])[C:6]=1[CH3:7].[CH2:15]([NH:17][CH2:18][CH3:19])[CH3:16]>CO>[Cl:14][C:11]1[CH:12]=[CH:13][C:3]2[CH:2]=[C:6]([CH2:7][N:17]([CH2:18][CH3:19])[CH2:15][CH3:16])[S:5](=[O:9])(=[O:8])[C:4]=2[CH:10]=1

Participants

4

Reactant 2

HCID 8021DiethylamineHCID 676224HCID 676224, compound

Product 1

HCID 67745068HCID 67745068, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 37.3 g (0.15 mol) 3,6-dichloro-2-methylbenzo[b]thiophene-1,1-dioxide, 200 ml methanol and 45 ml diethylamine is heated for 4 hours to reflux. Afterwards it is concentrated by evaporation, taken up in ethyl acetate, washed with water, dried, concentrated and chromatographed on silica gel (eluting agent ethyl acetate/isohexane 1:1). 29.5 g of the title compound (62% of the theoretical yield) having a melting point of 58°-59° C. is isolated.

Workup

  1. temperatureis heated for 4 hours
  2. temperatureto reflux
  3. concentrationAfterwards it is concentrated by evaporation
  4. washwashed with water
  5. customdried
  6. concentrationconcentrated
  7. customchromatographed on silica gel (eluting agent ethyl acetate/isohexane 1:1)

Sources & evidence

ORD record
ord-6a2e228b90554ceab09dc0736ab53c68
Source dataset
uspto-grants-1996_08
Patent number
US05547980

Reaction notes

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