Methanol → HCID 136333470, compound

HRID 915953Notes

Reaction equation

HRID 915953 reaction equation
CO.[CH:3]1([C:9]2[C:17]3[C:16](=[O:18])[NH:15][C:14]([C:19]4[CH:24]=[CH:23][C:22]([N:25]5[CH2:31][CH2:30][CH2:29][NH:28][CH2:27][CH2:26]5)=[CH:21][C:20]=4[O:32][CH3:33])=[N:13][C:12]=3[N:11]([CH3:34])[N:10]=2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]>CCOCC>[CH3:35][S:36]([OH:39])(=[O:38])=[O:37].[CH:3]1([C:9]2[C:17]3[C:16](=[O:18])[NH:15][C:14]([C:19]4[CH:24]=[CH:23][C:22]([N:25]5[CH2:31][CH2:30][CH2:29][NH:28][CH2:27][CH2:26]5)=[CH:21][C:20]=4[O:32][CH3:33])=[N:13][C:12]=3[N:11]([CH3:34])[N:10]=2)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]1

Participants

5

Reactant 3

HCID 887MethanolHCID 6395Methanesulfonic AcidHCID 136005859HCID 136005859, compound

Product 1

HCID 136333470HCID 136333470, compoundYield 69%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

To a 2 ml methanol solution of 74 mg (0.17 mmol) of the compound obtained in Example 133, 11.2 μl (0.17 mmol) of methanesulfonic acid was added, and the mixture was heated under reflux for 10 minutes. Then, the temperature of the reaction mixture was gradually lowered to room temperature. Ether was added to the resulting solution, and precipitated solids were collected by filtration to obtain 62 mg (69%) of the captioned compound.

Workup

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 10 minutes
  3. customwas gradually lowered to room temperature
  4. customprecipitated solids
  5. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-7c717cbe1258457780e9497f56d57492
Source dataset
uspto-grants-2007_09
Patent number
US07268128B2

Reaction notes

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