Hydrogen chloride-ethyl acetate → HCID 178482594, compound

HRID 554452Notes

Reaction equation

HRID 554452 reaction equation
[CH3:1][N:2]([CH2:10][C:11]1[CH:15]=[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:13]([S:22]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([C:31]3[NH:35][N:34]=[N:33][N:32]=3)[CH:26]=2)(=[O:24])=[O:23])[CH:12]=1)C(=O)OC(C)(C)C.C(OCC)(=O)C.[ClH:42]>CO>[ClH:42].[CH3:1][NH:2][CH2:10][C:11]1[CH:15]=[C:14]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:13]([S:22]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([C:31]3[NH:32][N:33]=[N:34][N:35]=3)[CH:26]=2)(=[O:24])=[O:23])[CH:12]=1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 178482595HCID 178482595, compound

Product 1

HCID 178482594HCID 178482594, compoundYield 86%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
65 °C

Procedure

To a solution (10 mL) of tert-butyl methyl[(5-phenyl-1-{[3-(1H-tetrazol-5-yl)phenyl]sulfonyl}-1H-pyrrol-3-yl)methyl]carbamate (52 mg) in methanol was added 4 mol/L hydrogen chloride-ethyl acetate solution (2 ml), and the mixture was stirred at 65° C. for 1.5 hr and concentrated under reduced pressure. The residue was crystallized from ethyl acetate to give the title compound as crystals (yield 42 mg, 86%).

Workup

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was crystallized from ethyl acetate

Sources & evidence

ORD record
ord-f5da7c7b67bf415f95eefd6c5e636eb0
Source dataset
uspto-grants-2011_11
Patent number
US08048909B2

Reaction notes

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