Methanesulfonic Acid → HCID 136342088, compound

HRID 915955Notes

Reaction equation

HRID 915955 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][N:26]([CH3:29])[CH2:25][CH2:24]5)=[CH:19][C:18]=4[O:30][CH:31]([F:33])[F:32])=[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]>CO>[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][N:26]([CH3:29])[CH2:25][CH2:24]5)=[CH:19][C:18]=4[O:30][CH:31]([F:32])[F: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 136005864HCID 136005864, compound

Product 1

HCID 136342088HCID 136342088, compoundYield 20.4%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A 2 ml methanol suspended solution of 65 mg (0.138 mmol) of the compound obtained in Example 138 was heated to 50° C. To the system, 9.1 μl (0.14 mmol) of methanesulfonic acid was added, and then the mixture was heated under reflux for 15 minutes. Then, the reaction mixture was brought to room temperature, and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate-ethanol to obtain 16 mg (20%) of the captioned compound.

Workup

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 15 minutes
  3. customwas brought to room temperature
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was recrystallized from ethyl acetate-ethanol

Sources & evidence

ORD record
ord-28154bd2fba94724bc4c2b16947d12f8
Source dataset
uspto-grants-2007_09
Patent number
US07268128B2

Reaction notes

Loading…