Chloroform → 2-Methoxymethyl-5-ethyl-5-methyl-1,3-dioxane

HRID 359944

반응식

HRID 359944 반응식
[CH2:1]([C:3]([CH3:8])([CH2:6][OH:7])[CH2:4][OH:5])[CH3:2].[CH3:9][O:10][CH2:11][CH:12]=O.C(Cl)(Cl)Cl.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>O>[CH3:9][O:10][CH2:11][CH:12]1[O:7][CH2:6][C:3]([CH2:1][CH3:2])([CH3:8])[CH2:4][O:5]1

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 661692-Ethyl-2-methyl-1,3-propanediolHCID 91563MethoxyacetaldehydeHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)

생성물 1

HCID 145979432-Methoxymethyl-5-ethyl-5-methyl-1,3-dioxane수율 89%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 590 g (5 moles) of 2-ethyl-2-methyl1,3-propanediol, 479 g (5.5 moles) of 85% strength methoxyacetaldehyde and 500 ml of chloroform was heated with 10 g of pyridinium p-toluenesulfonate under a water separator until water no longer separated off. The remaining solution was deionized using a mixed-bed ion exchanger, the solvent was removed under reduced pressure and the residue was distilled. 774 g (89% yield) of 2-methoxymethyl-5-ethyl-5-methyl-1,3-dioxane of boiling point 58° C./1 mbar were obtained.

후처리

  1. customno longer separated off
  2. customthe solvent was removed under reduced pressure
  3. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-3403804319c2480286773f5eb72da6c8
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05003089

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