HCID 54429385, compound → HCID 53945989, compound

HRID 1587552Notes

Reaction equation

HRID 1587552 reaction equation
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([N:9](S(C2C=CC(C)=CC=2)(=O)=O)[CH2:10][CH2:11][CH2:12][N:13](C(OC(C)(C)C)=O)[CH2:14][CH2:15][CH2:16][N:17]([C:28]2[CH:33]=[CH:32][C:31]([S:34][CH3:35])=[CH:30][CH:29]=2)S(C2C=CC(C)=CC=2)(=O)=O)=[CH:5][CH:4]=1>Br>[CH3:35][S:34][C:31]1[CH:30]=[CH:29][C:28]([NH:17][CH2:16][CH2:15][CH2:14][NH:13][CH2:12][CH2:11][CH2:10][NH:9][C:6]2[CH:7]=[CH:8][C:3]([S:2][CH3:1])=[CH:4][CH:5]=2)=[CH:33][CH:32]=1

Participants

3

Reactant 1

HCID 54429385HCID 54429385, compound

Product 1

HCID 53945989HCID 53945989, compound

Reagents, catalysts & solvents 1

HCID 260Hydrogen BromideSolvent

Procedure

Dissolve 1,9-bis(4-methylmercaptophenyl)-1,9-bis[(4-methylphenyl)sulfonyl]-5-(t-butyloxycarbonyl)-1,5,9-triazanonane (783 mg, 1 mmol) in 48% hydrobromic acid (mL). Stir for several hours and evaporate the solvent in vacuo. Dissolve the residue in water and neutralize with saturated sodium hydrogen carbonate and extract with ethyl acetate. Dry (MgSO4) and evaporate the solvent in vacuo. Purify by silica gel chromatography to give the title compound.

Workup

  1. customevaporate the solvent in vacuo
  2. dissolutionDissolve the residue in water
  3. extractionextract with ethyl acetate
  4. dry with materialDry (MgSO4)
  5. customevaporate the solvent in vacuo
  6. customPurify by silica gel chromatography

Sources & evidence

ORD record
ord-9e668b7b5a2a458d92123ae2b610dda3
Source dataset
uspto-grants-1993_06
Patent number
US05217964

Reaction notes

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