Methanol → HCID 67184742, compound

HRID 1958688Notes

Reaction equation

HRID 1958688 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[S:13][C:12]([C:14]([O:16]C)=[O:15])=[CH:11][C:10]=1[C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][CH2:27][O:28][CH:29]2[CH2:34][CH2:33][CH2:32][CH2:31][O:30]2)=[CH:20][CH:19]=1.[OH-].[Na+].CO>O>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[S:13][C:12]([C:14]([OH:16])=[O:15])=[CH:11][C:10]=1[C:18]1[CH:19]=[CH:20][C:21]([O:24][CH2:25][CH2:26][CH2:27][O:28][CH:29]2[CH2:34][CH2:33][CH2:32][CH2:31][O:30]2)=[CH:22][CH:23]=1

Participants

5

Reactant 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 67299344HCID 67299344, compound

Product 1

HCID 67184742HCID 67184742, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

3.1 g of the compound obtained in stage 16F) and then 800 mg of sodium hydroxide pellets are added to 30 ml of methanol and 1 ml of water. The reaction mixture is brought to reflux for 2 hours. It is concentrated to dryness, the residue is taken up in 500 ml of buffer solution at pH 2, extraction is carried out with ether and the extract is dried and concentrated to dryness. 3 g of the expected compound, crystallized from pentane, are obtained.

Workup

  1. temperatureto reflux for 2 hours
  2. concentrationIt is concentrated to dryness
  3. extractionthe residue is taken up in 500 ml of buffer solution at pH 2, extraction
  4. customthe extract is dried
  5. concentrationconcentrated to dryness
  6. custom3 g of the expected compound, crystallized from pentane
  7. customare obtained

Sources & evidence

ORD record
ord-279b3c97a6a5456da9136aa3e17705c0
Source dataset
uspto-grants-2013_04
Patent number
US08410137B2

Reaction notes

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