Methanesulfonic Acid → HCID 86745584, compound

HRID 1720778Notes

Reaction equation

HRID 1720778 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-5c2173e83f04426ebccd3ac062d8e629
Source dataset
uspto-grants-1996_04
Patent number
US05506354

Reaction notes

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