Ethane, 2-bromo-1,1-diethoxy- → HCID 21493040, compound

HRID 1973150Notes

Reaction equation

HRID 1973150 reaction equation
[S:1]([NH2:5])([NH2:4])(=[O:3])=[O:2].C(O[CH:9](OCC)[CH2:10][Br:11])C>Cl>[Br:11][CH2:10][CH:9]1[NH:5][S:1](=[O:3])(=[O:2])[NH:4][CH:9]([CH2:10][Br:11])[NH:5][S:1](=[O:3])(=[O:2])[NH:4]1

Participants

4

Reactant 2

HCID 74852Ethane, 2-bromo-1,1-diethoxy-HCID 82267Sulfamide

Product 1

HCID 21493040HCID 21493040, compoundYield 60%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

0.01 mole of sulphamide in 5 ml of concentrated hydrochloric acid is added to 0.012 mole of bromoacetaldehyde-diethylacetal, 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-(bromomethyl)-1,5-dithia-2,4,6,8-tetra-aza-cyclooctane-1,1,5,5-tetraoxide is obtained as colourless needle-shaped crystals of melting point 172° C (decomposition) in a yield of 60%.

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-867b16bbec34476ebd1074dc0b838596
Source dataset
uspto-grants-1976_12
Patent number
US03996242

Reaction notes

Loading…