Sodium Hydroxide → HCID 18947206, compound

HRID 1769156Notes

Reaction equation

HRID 1769156 reaction equation
[CH3:1][N:2]([CH3:15])[C:3]1([CH2:13][OH:14])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2S[CH2:5][CH2:4]1.[S:16]([O-:21])(O[O-])(=O)=[O:17].[K+].[K+].[OH-].[Na+]>O>[CH3:15][N:2]([CH3:1])[C:3]1([CH2:13][OH:14])[C:8]2[CH:7]=[CH:12][CH:11]=[CH:10][C:9]=2[S:16](=[O:21])(=[O:17])[CH2:5][CH2:4]1

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 10313463Potassium peroxymonosulphateHCID 18947221HCID 18947221, compound

Product 1

HCID 18947206HCID 18947206, compoundYield 50.1%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

10 g of 4-dimethylamino-4-hydroxymethyl-2,3-dihydro-4H-1-benzothiopyran obtained in Example 6 were suspended in 100 ml of water, to which 50 ml of an aqueous solution of 20 g of potassium peroxomonosulfate was added while stirring under ice cooling. After allowing to react for 1 hour, 3N NaOH solution was added thereto for neutralizing the mixture, followed by extraction with ether. After the ether phase was dried with anhydrous magnesium sulfate, the solvent was condensed to obtain 5.73 g of the title compound as colorless crystals. ##STR34## Melting point: 137°-138° C. IR(KBr) cm-1 : 1290, 1130, 760

Workup

  1. additionwas added
  2. customto react for 1 hour
  3. extractionfollowed by extraction with ether
  4. dry with materialAfter the ether phase was dried with anhydrous magnesium sulfate
  5. customcondensed

Sources & evidence

ORD record
ord-ac8ae49f553d40cf8bc476f220a3889b
Source dataset
uspto-grants-1995_01
Patent number
US05380748

Reaction notes

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