Sulfamide → HCID 118354476, compound

HRID 590559Notes

Reaction equation

HRID 590559 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][NH:11][CH:10]([CH2:14][NH2:15])[CH2:9]1)=O)(C)(C)C.[S:16](N)(N)(=[O:18])=[O:17]>N1C=CC=CC=1>[S:16]1(=[O:18])(=[O:17])[N:11]2[CH:10]([CH2:9][NH:8][CH2:13][CH2:12]2)[CH2:14][NH:15]1

Participants

4

Reactant 2

HCID 82267SulfamideHCID 53413950tert-Butyl 3-(aminomethyl)piperazine-1-carboxylate

Product 1

HCID 118354476HCID 118354476, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
150 °C

Procedure

To a stirred solution of 3-aminomethyl-piperazine-1-carboxylic acid tert-butyl ester (CAS number: 1376099-80-7, Bepharm) (215 mg, 1.0 mmol) in 2 mL of pyridine was added sulfamide (1.5 mmol). The reaction mixture was heated to 150° C. for 6 hours under microwave. The solvent was removed in vacuo, and the residue was dissolved in 3 mL of dichloromethane and 1 mL of TFA. The reaction mixture was stirred for 1 hour, and the solvent was removed in vacuo to give the crude Compound P which was used directly without further purification. LC/MS: calc'd 178 (MH+), measured 178 (MH+).

Workup

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in 3 mL of dichloromethane
  3. customthe solvent was removed in vacuo

Sources & evidence

ORD record
ord-58e9cab5677844298fc762534efc032d
Source dataset
uspto-grants-2016_01
Patent number
US09233978B2

Reaction notes

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