Methanesulfonic Acid → HCID 178485753, compound

HRID 1290078Notes

Reaction equation

HRID 1290078 reaction equation
[CH:1]1([CH2:7][C@H:8]([NH:19][C:20](=[O:49])[C@H:21]([CH2:43][C:44]2[N:48]=[CH:47][NH:46][CH:45]=2)[N:22]([CH3:42])[C:23](=[O:41])[C@H:24]([CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[NH:25][C:26]([N:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)=[O:27])[C@@H:9]([OH:18])[CH2:10][C@H:11]2[C:15]([CH3:17])([CH3:16])[O:14][CH2:13][O:12]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:50][S:51]([OH:54])(=[O:53])=[O:52]>C(OCC)(=O)C.C(O)C>[CH3:50][S:51]([OH:54])(=[O:53])=[O:52].[CH:1]1([CH2:7][C@H:8]([NH:19][C:20](=[O:49])[C@H:21]([CH2:43][C:44]2[N:48]=[CH:47][NH:46][CH:45]=2)[N:22]([CH3:42])[C:23](=[O:41])[C@H:24]([CH2:34][C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[NH:25][C:26]([N:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)=[O:27])[C@@H:9]([OH:18])[CH2:10][C@H:11]2[C:15]([CH3:17])([CH3:16])[O:14][CH2:13][O:12]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

5

Reactant 2

HCID 6395Methanesulfonic AcidHCID 178485751HCID 178485751, compound

Product 1

HCID 178485753HCID 178485753, compoundYield 82.5%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent2×

Procedure

The compound (310 mg) obtained in Example 1 was dissolved in ethyl acetate (7 ml) and a solution of methanesulfonic acid (44 mg) in ethyl acetate (5 ml) and ethanol (0.25 ml) was dropwise added. After stirring at room temperature for 3 hours, crystals were collected by filtration and dried under reduced pressure to give 292 mg of the title compound as white crystals (see Table 16).

Workup

  1. filtrationcrystals were collected by filtration
  2. customdried under reduced pressure

Sources & evidence

ORD record
ord-0154a20d7b3042f2a22beff0c0920b96
Source dataset
uspto-grants-1998_05
Patent number
US05750696

Reaction notes

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