Dimethyl Sulfoxide → HCID 131724696, compound

HRID 1759670Notes

Reaction equation

HRID 1759670 reaction equation
[CH3:1][S:2]([CH3:4])=[O:3].ClCCl.C(#N)C.[CH3:11][C:12]([CH3:23])([CH3:22])/[C:13](/[OH:21])=[CH:14]/[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])=[O:16].[CH3:24][C:25]([CH3:36])([CH3:35])/[C:26](/[OH:34])=[CH:27]/[C:28]([C:30]([CH3:33])([CH3:32])[CH3:31])=[O:29].[CH3:37][C:38]([CH3:49])([CH3:48])/[C:39](/[OH:47])=[CH:40]/[C:41]([C:43]([CH3:46])([CH3:45])[CH3:44])=[O:42].[Tb:50]>ClCCl.C(#N)C>[CH3:11][C:12]([CH3:23])([CH3:22])/[C:13](/[OH:21])=[CH:14]/[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])=[O:16].[CH3:24][C:25]([CH3:36])([CH3:35])/[C:26](/[OH:34])=[CH:27]/[C:28]([C:30]([CH3:33])([CH3:32])[CH3:31])=[O:29].[CH3:37][C:38]([CH3:49])([CH3:48])/[C:39](/[OH:47])=[CH:40]/[C:41]([C:43]([CH3:46])([CH3:45])[CH3:44])=[O:42].[Tb:50].[CH3:1][S:2]([CH3:4])=[O:3]

Participants

6

Reactant 4

HCID 679Dimethyl Sulfoxide2×HCID 6342AcetonitrileHCID 6344DichloromethaneHCID 6103705HCID 6103705, compound

Product 1

HCID 131724696HCID 131724696, compound

Reagents, catalysts & solvents 1

HCID 21877088Acetonitrile methylene chlorideSolvent2×

Procedure

1.0 mmole of dimethyl sulfoxide is dissolved in dichloromethane/acetonitrile solution, wherein the mole ratio for dichloromethane to acetonitrile is 1:1. Thereafter, the dichloromethane/acetonitrile solution that comprises the dimethyl sulfoxide is placed in a reactor. 1.0 mmole of (tri(2,2,6,6-tetramethyl-3,5-heptanedionate) Tb(III), Tb(TMHD)3 is also placed in the reactor, and a nitrogen gas is introduced into the reactor. The solution is subjected to thermal reflux for 2 hours and is then cooled to room temperature. Thereafter, the solvent is extracted with a rotary vacuum evaporator until the final volume of the solution is half of the original volume and when sediment is formed. After filtering the sediment, the filtered sediment is re-crystallized with methylcyclohexane to obtain the Tb(TMHD)3—DMSO) complex compound.

Workup

  1. customis placed in a reactor
  2. additiona nitrogen gas is introduced into the reactor
  3. temperaturethermal reflux for 2 hours
  4. extractionThereafter, the solvent is extracted with a rotary vacuum evaporator until the final volume of the solution
  5. customwhen sediment is formed
  6. filtrationAfter filtering the sediment
  7. customthe filtered sediment is re-crystallized with methylcyclohexane

Sources & evidence

ORD record
ord-a5707de104ab4701846526256d5d08bf
Source dataset
uspto-grants-2005_01
Patent number
US06838019B2

Reaction notes

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