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Triethylamine → 4-Methylsulfonyloxymethyl-1,3-dioxane

HRID 355271
Notes
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Reaction equation

HRID 355271 reaction equation
[O:1]1[CH2:6][CH2:5][CH:4]([CH2:7][OH:8])[O:3][CH2:2]1.C(N(CC)CC)C.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>C(Cl)Cl>[CH3:16][S:17]([O:8][CH2:7][CH:4]1[CH2:5][CH2:6][O:1][CH2:2][O:3]1)(=[O:19])=[O:18]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 13976559(1,3-Dioxan-4-yl)methanol

Product 1

HCID 189416164-Methylsulfonyloxymethyl-1,3-dioxaneYield 67.3%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A stirred solution of 16.2 grams (0.137 mole) of 1,3-dioxan-4-ylmethanol and 16.7 grams (0.165 mole) of triethylamine in 250 mL of methylene chloride was cooled to about -20° C., and a solution of 17.3 grams (0.151 mole) of methanesulfonyl chloride in about 25 mL of methylene chloride was added dropwise. Upon completion of addition the reaction mixture was allowed to warm to ambient temperature as it stirred for one hour. The reaction mixture was then washed with water and dried with magnesium sulfate. The mixture was filtered and concentrated under reduced pressure to a residue. The residue was purified using column chromatography on silica gel, yielding 18.1 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.

Workup

  1. additionUpon completion of addition the reaction mixture
  2. washThe reaction mixture was then washed with water
  3. dry with materialdried with magnesium sulfate
  4. filtrationThe mixture was filtered
  5. concentrationconcentrated under reduced pressure to a residue
  6. customThe residue was purified

Sources & evidence

ORD record
ord-18e8703d02b2465b8467d4e10992f5b4
Source dataset
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
USH0001759

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes