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Methyl iodide → (4R)-4,5-Dihydro-2-(methylthio)-4-thiazolemethanol

HRID 1957376
Notes
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Reaction equation

HRID 1957376 reaction equation
[OH:1][CH2:2][C@@H:3]1[CH2:7][S:6][C:5]([SH:8])=[N:4]1.[CH:9](N(C(C)C)CC)(C)C.CI>CO>[OH:1][CH2:2][C@@H:3]1[CH2:7][S:6][C:5]([S:8][CH3:9])=[N:4]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6328Methyl iodideHCID 81531DiisopropylethylamineHCID 178521049HCID 178521049, compound2×

Product 1

HCID 22862349(4R)-4,5-Dihydro-2-(methylthio)-4-thiazolemethanolYield 59%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a mixture solution of 4.88 g of 4(R)-hydroxymethyl-2-mercapto-1,3-thiazoline [Compound (5)] and 22.8 ml of diisopropylethylamine in 65 ml of dry methanol was added 14.00 g of methyl iodide under refluxing condition, and the reaction mixture was refluxed for 1 hour. After removal of the solvent under reduced pressure, the resulting residue was dissolved in ethyl acetate and the organic layer was washed with saturated sodium bicarbonate solution, water and saturated saline solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and the resulting residue was purified by silica gel column chromatography (chloroform-acetone) to give 3.14 g (59%) of 4(R)-hydroxymethyl-2-methylthio-1,3-thiazoline [Compound (6)].

Workup

  1. temperatureunder refluxing condition
  2. temperaturethe reaction mixture was refluxed for 1 hour
  3. customAfter removal of the solvent under reduced pressure
  4. dissolutionthe resulting residue was dissolved in ethyl acetate
  5. washthe organic layer was washed with saturated sodium bicarbonate solution, water and saturated saline solution
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customthe resulting residue was purified by silica gel column chromatography (chloroform-acetone)

Sources & evidence

ORD record
ord-060f4bd975894dc8a351c241cc99c3fa
Source dataset
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05783703

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes