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Triethylamine → 4-Methylsulfonyloxymethyl-1,3-dioxane

HRID 355271
ノート
印刷プレビュー

反応式

HRID 355271 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 189416164-Methylsulfonyloxymethyl-1,3-dioxane収率 67.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-18e8703d02b2465b8467d4e10992f5b4
出典データセット
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USH0001759

反応ノート

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