Methanesulfonic Acid → HCID 86750179, compound

HRID 233516Notes

Reaction equation

HRID 233516 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[OH:6][C@@H:7]1[C@@H:26]([N:27]2[CH2:32][CH2:31][S:30][C:29]([CH3:34])([CH3:33])[CH2:28]2)[CH2:25][C@@:24]2([CH3:35])[C@@H:9]([CH2:10][CH2:11][C@@H:12]3[C@@H:23]2[CH2:22][CH2:21][C@@:20]2([CH3:36])[C@H:13]3[CH2:14][CH2:15][C@@H:16]2[C:17](=[O:19])[CH3:18])[CH2:8]1>CO>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[OH:6][C@@H:7]1[C@@H:26]([N:27]2[CH2:32][CH2:31][S:30][C:29]([CH3:34])([CH3:33])[CH2:28]2)[CH2:25][C@@:24]2([CH3:35])[C@@H:9]([CH2:10][CH2:11][C@@H:12]3[C@@H:23]2[CH2:22][CH2:21][C@@:20]2([CH3:36])[C@H:13]3[CH2:14][CH2:15][C@@H:16]2[C:17](=[O:19])[CH3:18])[CH2:8]1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 10813342HCID 10813342, compound

Product 1

HCID 86750179HCID 86750179, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

A solution of methanesulfonic acid (100 mg) in methanol (20 ml) was added to a solution of (2β,3α,5α)-3-hydroxy-2-(2,2-dimethyl-4-thiomorpholinyl)pregnan-20-one (464 mg) in methanol (30 ml). The solvent was removed under reduced pressure and the residue was crystallised from acetone to give (2β,3α,5α)-3-hydroxy-2-(2,2-dimethyl-4-thiomorpholinyl)pregnan-20-one methanesulfonate (1:1) salt (337 mg). m.p. 171°-177° C.; [α]D +104.6° (c 0.9).

Workup

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was crystallised from acetone

Sources & evidence

ORD record
ord-3967da4af97c43b5b64c35008dcb683e
Source dataset
uspto-grants-1997_01
Patent number
US05593983

Reaction notes

Loading…