Isopropanol → Acrylic Acid 1-allyloxy-2-propanol

HRID 1651495

反応式

HRID 1651495 の反応式
C(O)(C)C.[C:5]([OH:9])(=[O:8])[CH:6]=[CH2:7].[CH2:10]([O:13][CH2:14][CH:15]([OH:17])[CH3:16])[CH:11]=[CH2:12].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+]>O>[C:5]([OH:9])(=[O:8])[CH:6]=[CH2:7].[CH2:10]([O:13][CH2:14][CH:15]([OH:17])[CH3:16])[CH:11]=[CH2:12]

参加物

6

反応物 4

HCID 3776IsopropanolHCID 6581Acrylic AcidHCID 62655Sodium PersulfateHCID 5421782-Propanol, 1-(2-propenyloxy)-

生成物 1

HCID 86743966Acrylic Acid 1-allyloxy-2-propanol

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
40 °C

実験手順

A suitable reaction flask was equipped with a mechanical agitator, a thermometer, a reflux condenser, a nitrogen inlet and two addition inlets for the initiator and monomer solutions. The flask was charged with 170 g of deionized water and 30 g of isopropanol. The resulting solution was then heated to reflux under a nitrogen blanket. 43.2 g of acrylic acid (0.6 mole) and 23.2 g of 1-allyloxy-2-propanol [AOP] (94% pure, 0.19 mole) were mixed in a separate flask so as to provide a mixed monomer solution. The mixed monomer solution was then transferred to an addition funnel. An initiator solution containing 24.4% of sodium persulfate in deionized water was prepared separately and sparged with nitrogen. The initiator solution (17 g) was then added to the reaction flask along with the mixed monomer solution over a period of two hours. After this addition, some addition persulfate solution was added to the reaction mixture for one more hour at 85° C. and, subsequently, 90.0 g of the isopropanol/water solution were stripped off. The reaction mixture was then cooled to lower than 40° C. and 36 g of 50% caustic solution was then added.

後処理

  1. customA suitable reaction flask was equipped with a mechanical agitator
  2. additiona thermometer, a reflux condenser, a nitrogen inlet and two addition inlets for the initiator and monomer solutions
  3. temperatureThe resulting solution was then heated
  4. temperatureto reflux under a nitrogen blanket
  5. customto provide a mixed monomer solution
  6. customThe mixed monomer solution was then transferred to an addition funnel
  7. customwas prepared separately
  8. customsparged with nitrogen
  9. additionThe initiator solution (17 g) was then added to the reaction flask along with the mixed monomer solution over a period of two hours
  10. additionAfter this addition
  11. additionsome addition persulfate solution
  12. additionwas added to the reaction mixture for one more hour at 85° C.
  13. addition36 g of 50% caustic solution was then added

出典と根拠

ORDレコード
ord-ea64ae1bd84b4b06aca3fb4ef81f8b1b
出典データセット
uspto-grants-1990_05
特許番号
US04929362

関連ノート

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