Methanesulfonic Acid → HCID 136333176, compound

HRID 915966Notes

Reaction equation

HRID 915966 reaction equation
[CH:1]1([C:7]2[C:15]3[C:14](=[O:16])[NH:13][C:12]([C:17]4[CH:22]=[CH:21][C:20]([N:23]5[CH2:28][CH2:27][CH:26]([N:29]([CH3:31])[CH3:30])[CH2:25][CH2:24]5)=[CH:19][C:18]=4[O:32][CH3:33])=[N:11][C:10]=3[N:9]([CH3:34])[N:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]>C(O)C>[CH3:35][S:36]([OH:39])(=[O:38])=[O:37].[CH:1]1([C:7]2[C:15]3[C:14](=[O:16])[NH:13][C:12]([C:17]4[CH:22]=[CH:21][C:20]([N:23]5[CH2:28][CH2:27][CH:26]([N:29]([CH3:30])[CH3:31])[CH2:25][CH2:24]5)=[CH:19][C:18]=4[O:32][CH3:33])=[N:11][C:10]=3[N:9]([CH3:34])[N:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 136005798HCID 136005798, compound

Product 1

HCID 136333176HCID 136333176, compoundYield 46.2%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a 1 ml ethanol solution of 50 mg (0.108 mmol) of the compound obtained in Example 153, 7.1 ml (0.110 mmol) of methanesulfonic acid was added, and the mixture was heated under reflux for 10 minutes. Then, the reaction mixture was cooled to room temperature, and the solvent was distilled off under reduced pressure. The residue was purified by recrystallization (ethyl acetate-ethanol) to obtain 28 mg (46%) of the captioned compound.

Workup

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 10 minutes
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by recrystallization (ethyl acetate-ethanol)

Sources & evidence

ORD record
ord-071d15a04c9248008653455f5441f106
Source dataset
uspto-grants-2007_09
Patent number
US07268128B2

Reaction notes

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