Diethyl Carbonate → 5,5-Dimethyl-1,3-dioxan-2-one

HRID 905320

反応式

HRID 905320 の反応式
[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH2:3][OH:4].[C:8](=O)(OCC)[O:9]CC.O(C)[Na]>>[CH3:1][C:2]1([CH3:7])[CH2:5][O:6][C:8](=[O:9])[O:4][CH2:3]1

参加物

4

反応物 3

HCID 7766Diethyl CarbonateHCID 31344Neopentyl glycolHCID 178418582HCID 178418582、化合物

生成物 1

HCID 1379845,5-Dimethyl-1,3-dioxan-2-one

反応条件

温度
130 °C

実験手順

A mixture of 208 grams (2 moles) 2,2-dimethyl-1,3-propanediol (neopentyl glycol), 295 grams diethyl carbonate, and 4.3 grams NaOCH3 was placed in a flask equipped with an 18-inch vigreux column and heated gradually to 130° C. About 230 ml ethanol was distilled. When the pot temperature reached 150°-160° C. excess diethyl carbonate was removed under reduced pressure. The resulting product was dissolved in benzene, washed with water, and concentrated. This product was recrystallized from ether and isolated as pure 5,5-dimethyl-1,3-dioxan-2-one. A 75 gram sample had a melting point of 108° C., very nearly matching that in the literature (109° C.).

後処理

  1. customwas placed in a flask
  2. customequipped with an 18-inch vigreux column
  3. distillationAbout 230 ml ethanol was distilled
  4. customreached 150°-160° C.
  5. customwas removed under reduced pressure
  6. dissolutionThe resulting product was dissolved in benzene
  7. washwashed with water
  8. concentrationconcentrated
  9. customThis product was recrystallized from ether

出典と根拠

ORDレコード
ord-2efce97ef5984f6f988a33502bfa9cc4
出典データセット
uspto-grants-1983_12
特許番号
US04423205

関連ノート

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