Chloroacetaldehyde → HCID 21493045, compound

HRID 1973149Notes

Reaction equation

HRID 1973149 reaction equation
[S:1]([NH2:5])([NH2:4])(=[O:3])=[O:2].[Cl:6][CH2:7][CH:8]=O>Cl>[Cl:6][CH2:7][CH:8]1[NH:5][S:1](=[O:3])(=[O:2])[NH:4][CH:8]([CH2:7][Cl:6])[NH:5][S:1](=[O:3])(=[O:2])[NH:4]1

Participants

4

Reactant 2

HCID 33ChloroacetaldehydeHCID 82267Sulfamide

Product 1

HCID 21493045HCID 21493045, compoundYield 70%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

0.01 mole of sulphamide in 5 ml of concentrated hydrochloric acid are added to 0.012 mole of chloroacetaldehyde, at room temperature whilst stirring. After 5 minutes, the precipitate which has formed is filtered off and washed with ice water, dried and recrystallised from acetone/petroleum ether. 3,7-Di-(chloromethyl)-1,5-dithia-2,4,6,8-tetra-aza-cyclooctane-1,1,5,5-tetraoxide is obtained as colourless crystals of melting point 175° C (decomposition) in a yield of 70% of the theoretical yield.

Workup

  1. customthe precipitate which has formed
  2. filtrationis filtered off
  3. washwashed with ice water
  4. customdried
  5. customrecrystallised from acetone/petroleum ether

Sources & evidence

ORD record
ord-a4085e667849461f86a693df75142e02
Source dataset
uspto-grants-1976_12
Patent number
US03996242

Reaction notes

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