Methanesulfonic Acid → HCID 86672601, compound

HRID 470686Notes

Reaction equation

HRID 470686 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C@H:9]1[O:14][CH2:13][C@H:12]([NH:15][C:16]([C@@H:18]2[NH:32][C:31]3([CH2:37][CH2:36][C:35]([CH3:39])([CH3:38])[CH2:34][CH2:33]3)[C@:20]3([C:28]4[C:23](=[CH:24][C:25]([Cl:29])=[CH:26][CH:27]=4)[NH:22][C:21]3=[O:30])[C@H:19]2[C:40]2[CH:45]=[CH:44][N:43]=[C:42]([Cl:46])[C:41]=2[F:47])=[O:17])[CH2:11][CH2:10]1)(=[O:8])[NH2:7]>CC(O)C>[OH2:3].[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C@H:9]1[O:14][CH2:13][C@H:12]([NH:15][C:16]([C@@H:18]2[NH:32][C:31]3([CH2:33][CH2:34][C:35]([CH3:39])([CH3:38])[CH2:36][CH2:37]3)[C@:20]3([C:28]4[C:23](=[CH:24][C:25]([Cl:29])=[CH:26][CH:27]=4)[NH:22][C:21]3=[O:30])[C@H:19]2[C:40]2[CH:45]=[CH:44][N:43]=[C:42]([Cl:46])[C:41]=2[F:47])=[O:17])[CH2:11][CH2:10]1)(=[O:8])[NH2:7]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 73297272Milademetan

Product 1

HCID 86672601HCID 86672601, compoundYield 81.9%

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

Methanesulfonic acid (0.006 ml, 0.09 mmol) was added to a 2-propanol (0.5 ml) solution of the compound (54 mg, 0.09 mmol) obtained in Example 70 and the resulting mixture was dissolved by heating. After stirring at room temperature for 3 days, the precipitate was collected by filtration to give 27 mg (43%) of the title compound as a solid.

Workup

  1. dissolutionthe resulting mixture was dissolved
  2. temperatureby heating
  3. filtrationthe precipitate was collected by filtration

Sources & evidence

ORD record
ord-b44dbfa1e1a04975ba25ca13517edf71
Source dataset
uspto-grants-2014_01
Patent number
US08629133B2

Reaction notes

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