Methanesulfonic Acid → HCID 86745584, compound

HRID 1769530Notes

Reaction equation

HRID 1769530 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-8b8674df70d241399a26fa6660c3b9b4
Source dataset
uspto-grants-1995_01
Patent number
US05380841

Reaction notes

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