Methanesulfonic Acid → HCID 136333294, compound

HRID 915926Notes

Reaction equation

HRID 915926 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]([OH:29])[CH2:25][CH2:24]5)=[CH:19][C:18]=4[O:30][CH3:31])=[N:11][C:10]=3[N:9]([CH3:32])[N:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:33][S:34]([OH:37])(=[O:36])=[O:35]>C(O)C>[CH3:33][S:34]([OH:37])(=[O:36])=[O:35].[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]([OH:29])[CH2:25][CH2:24]5)=[CH:19][C:18]=4[O:30][CH3:31])=[N:11][C:10]=3[N:9]([CH3:32])[N:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 136005817HCID 136005817, compound

Product 1

HCID 136333294HCID 136333294, compoundYield 83%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
50 °C

Procedure

A 3 ml ethanol suspension of 100 mg (0.23 mmol) of the compound obtained in Example 31 was heated to 50° C. to form a solution. To this solution, 15 μM (0.23 mmol) of methanesulfonic acid was added, and the mixture was heated under reflux for 10 minutes. Then, the reaction mixture was brought to room temperature, and the solvent was distilled off under reduced pressure. Ether was added to the residue, and solids were collected by filtration to obtain 101 mg (83%) of the captioned compound.

Workup

  1. customto form a solution
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 10 minutes
  4. customwas brought to room temperature
  5. distillationthe solvent was distilled off under reduced pressure
  6. additionEther was added to the residue, and solids
  7. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-229a0b72d6984be8b89ffca668c86833
Source dataset
uspto-grants-2007_09
Patent number
US07268128B2

Reaction notes

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