Methanol → HCID 136333381, compound

HRID 915940Notes

Reaction equation

HRID 915940 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]([C:25]([N:27]5[CH2:32][CH2:31][N:30]([CH3:33])[CH2:29][CH2:28]5)=[O:26])=[CH:21][C:20]=4[O:34][CH3:35])=[N:13][C:12]=3[N:11]([CH3:36])[N:10]=2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.[CH3:37][S:38]([OH:41])(=[O:40])=[O:39]>CCOCC>[CH3:37][S:38]([OH:41])(=[O:40])=[O:39].[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]([C:25]([N:27]5[CH2:28][CH2:29][N:30]([CH3:33])[CH2:31][CH2:32]5)=[O:26])=[CH:21][C:20]=4[O:34][CH3:35])=[N:13][C:12]=3[N:11]([CH3:36])[N:10]=2)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]1

Participants

5

Reactant 3

HCID 887MethanolHCID 6395Methanesulfonic AcidHCID 136005862HCID 136005862, compound

Product 1

HCID 136333381HCID 136333381, compoundYield 81%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

To a 1 ml methanol/1 ml tetrahydrofuran mixed solution of 45 mg (0.097 mmol) of the compound obtained in Example 66, 6.4 μl (0.098 mmol) of methanesulfonic acid was added, and the mixture was stirred at room temperature for 10 minutes. Ether was added to the resulting solution, and precipitated solids were collected by filtration, thereby obtaining 43.9 mg (81%) of the captioned compound.

Workup

  1. customprecipitated solids
  2. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-bf79734f966941ccad5413c6f36ca1f5
Source dataset
uspto-grants-2007_09
Patent number
US07268128B2

Reaction notes

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