Methanesulfonic Acid → HCID 86745584, compound

HRID 1769493Notes

Reaction equation

HRID 1769493 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-b2b9aab7c5574554a90fcf4754bd9fc1
Source dataset
uspto-grants-1995_01
Patent number
US05380840

Reaction notes

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