Methanesulfonic Acid → HCID 136333179, compound

HRID 915952Notes

Reaction equation

HRID 915952 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]([CH2:25][CH2:26][N:27]([CH3:29])[CH3:28])[CH3:24])=[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]>CO>[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]([CH2:25][CH2:26][N:27]([CH3:28])[CH3:29])[CH3:24])=[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 136005806HCID 136005806, compound

Product 1

HCID 136333179HCID 136333179, compoundYield 55.5%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A 2 ml methanol suspended solution of 130 mg (0.30 mmol) of the compound obtained in Example 131 was heated to 50° C. To the system, 20 μl (0.30 mmol) of methanesulfonic acid was added, and the temperature of the mixture was gradually lowered to room temperature. Then, the solvent was distilled off under reduced pressure, and the, residue was dissolved by addition of ethyl acetate. Ether was added to the resulting solution, and precipitated solids were collected by filtration to obtain 89 mg (55%) of the captioned compound.

Workup

  1. customwas gradually lowered to room temperature
  2. distillationThen, the solvent was distilled off under reduced pressure
  3. dissolutionthe, residue was dissolved by addition of ethyl acetate
  4. additionEther was added to the resulting solution
  5. customprecipitated solids
  6. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-6eb913c0410c4a7e94d6b01f42f31954
Source dataset
uspto-grants-2007_09
Patent number
US07268128B2

Reaction notes

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