Chloroform → 2,5-Dimethoxymethyl-5-methyl-1,3-dioxane

HRID 359945

反応式

HRID 359945 の反応式
[CH3:1][O:2][CH2:3][C:4]([CH3:9])([CH2:7]O)[CH2:5][OH:6].[CH3:10][O:11][CH2:12][CH:13]=[O:14].C(Cl)(Cl)Cl.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>O>[CH3:10][O:11][CH2:12][CH:13]1[O:6][CH2:5][C:4]([CH2:3][O:2][CH3:1])([CH3:9])[CH2:7][O:14]1

参加物

6

反応物 4

HCID 6212ChloroformHCID 888862-(Methoxymethyl)-2-methylpropane-1,3-diolHCID 91563MethoxyacetaldehydeHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)

生成物 1

HCID 145979442,5-Dimethoxymethyl-5-methyl-1,3-dioxane収率 91%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 670 g (5 moles) of 2-methoxymethyl2-methyl-1,3-propanediol, 479 g (5.5 moles) of 85% strength methoxyacetaldehyde and 250 ml of chloroform was heated with 10 g of pyridinium p-toluenesulfonate under a water separator until water no longer separated off. The solution was deionized using a mixed-bed ion exchanger, the solvent was stripped off under reduced pressure and the residue was subjected to fractional distillation under reduced pressure. 864 g (91% yield) of 2,5-dimethoxymethyl-5-methyl-1,3-dioxane of boiling point 95° C./10 mbar were obtained.

後処理

  1. customno longer separated off
  2. distillationthe residue was subjected to fractional distillation under reduced pressure

出典と根拠

ORDレコード
ord-88ff168f230848ee9c90174d2615cc11
出典データセット
uspto-grants-1991_03
特許番号
US05003089

関連ノート

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