4,4-Diethoxybutylamine → HCID 70270548, compound

HRID 1939853

Reaction equation

HRID 1939853 reaction equation
[CH2:1]([O:3][CH:4]([O:9][CH2:10][CH3:11])[CH2:5][CH2:6][CH2:7][NH2:8])[CH3:2].[S:12](Cl)([OH:15])(=O)=[O:13].[CH:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>>[CH2:10]([O:9][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][CH2:6][CH2:7][NH:8][S:12]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)(=[O:15])=[O:13])[CH3:11]

Participants

3

Reactant 2

HCID 806724,4-DiethoxybutylamineHCID 22564087Benzene sulphochloride

Product 1

HCID 70270548HCID 70270548, compoundYield 86%

Procedure

42 g 4-amino butyraldehyde diethyl acetal and 88 g benzene sulfochloride are processed as explained in Preparation Example 1. The reaction mixture is not clear from the very beginning and vigorous stirring is therefore indispensable. Methylene chloride is used for the extraction of the sulfonamide acetal. Yield: 86% based on the amino acetal used. The product will crystallize when standing for an extended time at room temperature; melting point: 109°-111°° C.; for further purification recrystallization from a 2:1 volume mixture of water and ethanol is possible.

Workup

  1. customas explained in Preparation Example 1
  2. extractionMethylene chloride is used for the extraction of the sulfonamide acetal
  3. customThe product will crystallize when
  4. customstanding for an extended time at room temperature
  5. customfor further purification recrystallization
  6. additionfrom a 2:1 volume mixture of water and ethanol

Sources & evidence

ORD record
ord-f479b9f1c492412d8f65bb6cdc580c4f
Source dataset
uspto-grants-1997_12
Patent number
US05698360

Linked notes

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