Trifluoroacetic acid methylene chloride → HCID 23130194, compound

HRID 1363865Notes

Reaction equation

HRID 1363865 reaction equation
C(OC([NH:8][S:9](=[O:26])(=[O:25])[O:10][CH2:11][CH2:12][NH:13][S:14]([NH:17]C(OC(C)(C)C)=O)(=[O:16])=[O:15])=O)(C)(C)C.FC(F)(F)C(O)=O.ClCCl>ClCCl>[S:9](=[O:26])(=[O:25])([O:10][CH2:11][CH2:12][NH:13][S:14]([NH2:17])(=[O:15])=[O:16])[NH2:8]

Participants

4

Reactant 2

HCID 21863450Trifluoroacetic acid methylene chlorideHCID 23130193HCID 23130193, compound

Product 1

HCID 23130194HCID 23130194, compoundYield 89.3%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
20 °C

Procedure

To 1.5 g of 2-({[(tert-butoxycarbonyl)amino]sulfonyl}amino)ethyl tert-butoxycarbonylsulfamate in 30 ml of dichloromethane are added 30 ml of a 1/1 trifluoroacetic acid/dichloromethane mixture. After stirring for 4 hours at 20° C., the reaction mixture is concentrated under reduced pressure and taken up 3 times in ether and reevaporated. The white solid is taken up in dichloromethane and filtered under vacuum to give 700 mg of the desired product: 2-[(aminosulfonyl)amino]ethyl sulfamate.

Workup

  1. concentrationthe reaction mixture is concentrated under reduced pressure
  2. customreevaporated
  3. filtrationfiltered under vacuum

Sources & evidence

ORD record
ord-b77aa2e871614a558d22057aacaf9ea3
Source dataset
uspto-grants-2011_02
Patent number
US07887824B2

Reaction notes

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