Methanesulfonic Acid → HCID 86745584, compound

HRID 1769464Notes

Reaction equation

HRID 1769464 reaction equation
[OH:1][C@:2]1([C@:34]2([CH3:35])[C@H:20]([C@H:21]3[C:31](=[CH:32][CH2:33]2)[C@:29]2([CH3:30])[C:24](=[CH:25][C:26](=[O:36])[CH2:27][CH2:28]2)[CH2:23][CH2:22]3)[CH2:19][CH2:18]1)[C:3](=[O:17])[CH2:4][N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[CH2:7][CH2:6]1.[CH3:37][S:38]([OH:41])(=[O:40])=[O:39]>CO>[CH3:37][S:38]([OH:41])(=[O:40])=[O:39].[OH:1][C@:2]1([C@:34]2([CH3:35])[C@H:20]([C@H:21]3[C:31](=[CH:32][CH2:33]2)[C@:29]2([CH3:30])[C:24](=[CH:25][C:26](=[O:36])[CH2:27][CH2:28]2)[CH2:23][CH2:22]3)[CH2:19][CH2:18]1)[C:3](=[O:17])[CH2:4][N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[CH2:7][CH2:6]1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 14307778HCID 14307778, compound

Product 1

HCID 86745584HCID 86745584, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

17α-Hydroxy-21-[4-(2-pyridinyl)-1-piperazinyl]pregna-4,9(11)-diene-3,20-dione (Example 1) is dissolved in methanol and treated with methane sulfonic acid (0.224 g). The solution is concentrated and the residue is crystallized from hot methanol and ethyl acetate to give a first crop of the title compound. A second crop of the mesylate is isolated.

Workup

  1. concentrationThe solution is concentrated
  2. customthe residue is crystallized from hot methanol and ethyl acetate

Sources & evidence

ORD record
ord-73ed2545fb4245b6931027fcc508f9df
Source dataset
uspto-grants-1995_01
Patent number
US05380839

Reaction notes

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