Ethylene Glycol → Non-8-en-2-one ethylene ketal

HRID 27311

반응식

HRID 27311 반응식
[CH3:1][C:2](=[O:10])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[CH2:9].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:23](O)[CH2:24][OH:25].C1C=CC=CC=1>O>[CH2:24]1[O:25][C:2]([CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[CH2:9])([CH3:1])[O:10][CH2:23]1

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 241BenzeneHCID 211088-Nonen-2-oneHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 25186484Non-8-en-2-one ethylene ketal수율 74.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution containing 119.0 g of non-8-en-2-one, (prepared in Example 22 B-3), 1.2 g p-toluenesulfonic acid monohydrate, 63.1 g of ethylene glycol and 420 ml anhydrous benzene was prepared and refluxed for about 15 to 17 hr. Water which formed was collected in a Dean-Stark trap. The solution was cooled to room temperature and 250 ml of 5% aqueous sodium bicarbonate solution was added thereto. The benzene layer was separated and dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was distilled to yield 116.8 g of title compound having the following physical characteristics:

후처리

  1. customwas prepared
  2. temperaturerefluxed for about 15 to 17 hr
  3. customwas collected in a Dean-Stark trap
  4. addition250 ml of 5% aqueous sodium bicarbonate solution was added
  5. customThe benzene layer was separated
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated in vacuo
  8. distillationThe residue was distilled

출처 및 근거

ORD 기록
ord-03d3c9a888364d9198fc5a1432e42bbf
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220795

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