Benzoic Acid → Vinylbenzoic acid

HRID 973905

반응식

HRID 973905 반응식
N#N.C([C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[CH:7][CH:6]=1)=C.[C:14](OCC=C)(=O)[C:15](C)=C.C(O)(=O)C1C=CC=CC=1.C(OC(=O)C(C)=C)CCCCCCCCCCC>C(OC(=O)C)C.O1CCCC1>[CH:14]([C:7]1[CH:6]=[CH:5][CH:13]=[CH:12][C:8]=1[C:9]([OH:11])=[O:10])=[CH2:15]

참가 물질

8

반응물 5

HCID 243Benzoic AcidHCID 947NitrogenHCID 7274Allyl methacrylateHCID 8906Lauryl MethacrylateHCID 140984-Vinylbenzoic acid

생성물 1

HCID 3015504Vinylbenzoic acid

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

반응 조건

온도
70 °C

실험 절차

Into a 500 ml. 2-necked flask fitted with a thermometer, and a reflux condenser connected to a N2 source, was introduced a mixture of 3.5 g of 4-vinylbenzoic acid (Aldrich Chemical Co. , 3 g of allyl methacrylate, 150 ml tetrahydrofuran and 150 ml ethylacetate. The mixture was stirred to dissolve the benzoic acid compound. Next was added 93.5 g of laurylmethacrylate. The flask was purged with N2 and heated at 70° C. for 10 minutes. The flask was purged again with N2 and 1 g of 2,2-azobisisobutyronitrile (AIBN) was added all at once and heated at 70° C. under a N2 blanket. This was continued for a period of 8 hours. The resulting polymeric solution was cooled to room temperature and diluted with twice its volume with Isopar™ G and filtered to remove insoluble materials (About 125 mg of homopolymer of VBA acid remained on the filter paper). The clear filtered polymeric solution was further diluted with Isopar™ G to 4.1 liters and was subjected to distillation under reduced pressure until about 500 ml of the distillate was collected in the receiving flask. The distillate was mainly ethylacetate, tetrahydrofuran and Isopar™ G).

후처리

  1. custom2-necked flask fitted with a thermometer, and a reflux condenser
  2. additionwas introduced
  3. customThe flask was purged with N2
  4. customThe flask was purged again with N2 and 1 g of 2,2-azobisisobutyronitrile (AIBN)
  5. additionwas added all at once and
  6. temperatureheated at 70° C. under a N2 blanket
  7. temperatureThe resulting polymeric solution was cooled to room temperature
  8. additiondiluted with twice its volume with Isopar™ G
  9. filtrationfiltered
  10. customto remove insoluble materials (About 125 mg of homopolymer of VBA acid
  11. additionThe clear filtered polymeric solution was further diluted with Isopar™ G to 4.1 liters
  12. distillationwas subjected to distillation under reduced pressure until about 500 ml of the distillate
  13. customwas collected in the receiving flask

출처 및 근거

ORD 기록
ord-f4a56db9433e4313ac9b26d3334542cb
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05066559

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