Methanesulfonic Acid → HCID 87481204, compound

HRID 732799Notes

Reaction equation

HRID 732799 reaction equation
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:12]([O:22][C:23]3[CH:28]=[CH:27][C:26]([O:29][CH2:30][CH2:31][N:32]4[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]4)=[CH:25][CH:24]=3)=[C:13]3[C:18](=[CH:19][CH:20]=2)[CH:17]=[C:16]([OH:21])[CH:15]=[CH:14]3)=[CH:7][CH:6]=1)(=[O:4])=[O:3].[CH3:38][S:39](O)(=[O:41])=[O:40]>C(OCC)(=O)C>[CH3:38][S:39]([O:21][C:16]1[CH:15]=[CH:14][C:13]2[C:18](=[CH:19][CH:20]=[C:11]([C:8]3[CH:7]=[CH:6][C:5]([S:2]([CH3:1])(=[O:4])=[O:3])=[CH:10][CH:9]=3)[C:12]=2[O:22][C:23]2[CH:28]=[CH:27][C:26]([O:29][CH2:30][CH2:31][N:32]3[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]3)=[CH:25][CH:24]=2)[CH:17]=1)(=[O:41])=[O:40]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 5327043648904-56-7

Product 1

HCID 87481204HCID 87481204, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

Heat approximately 1.0 g of the compound of Example 3 in a solvent mixture consisting of 3 mL of 3A-ethanol and 5 mL ethyl acetate to provide a thin slurry. Add methanesulfonic acid (185 mg) in 1 mL of 3A-ethanol to the hot slurry. Cool and stir for approximately 1 hour upon reaching room temperature. Filter the slurry and rinse with ethyl acetate. Vacuum dry the filter cake at 45° C. over 2-3 days to recover approximately 1.11 g of the title compound.

Workup

  1. customto provide a thin slurry
  2. temperatureCool
  3. customupon reaching room temperature
  4. filtrationFilter the slurry
  5. washrinse with ethyl acetate
  6. customVacuum dry the filter cake at 45° C. over 2-3 days
  7. customto recover approximately 1.11 g of the title compound

Sources & evidence

ORD record
ord-12147bc461194cf0a2dfd34bb57fa0d2
Source dataset
uspto-grants-2009_09
Patent number
US07585977B2

Reaction notes

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