1,4-Butanediol monovinyl ether → Bis(4-vinyloxybutyl) fumarate

HRID 1823641

반응식

HRID 1823641 반응식
[C:1]([O:9][CH3:10])(=[O:8])/[CH:2]=[CH:3]/[C:4]([O:6][CH3:7])=[O:5].[CH:11]([O:13][CH2:14][CH2:15][CH2:16]CO)=[CH2:12]>C([O-])(=O)C.[Zn+2].C([O-])(=O)C.CC(C1C(O)=C(C(C)(C)C)C=C(CCC(OCC(COC(CCC2C=C(C(C)(C)C)C(O)=C(C(C)(C)C)C=2)=O)(COC(CCC2C=C(C(C)(C)C)C(O)=C(C(C)(C)C)C=2)=O)COC(CCC2C=C(C(C)(C)C)C(O)=C(C(C)(C)C)C=2)=O)=O)C=1)(C)C.CO>[C:1]([O:9][CH2:10][CH2:16][CH2:15][CH2:14][O:13][CH:11]=[CH2:12])(=[O:8])/[CH:2]=[CH:3]/[C:4]([O:6][CH2:7][CH2:16][CH2:15][CH2:14][O:13][CH:11]=[CH2:12])=[O:5]

참가 물질

6

반응물 2

HCID 873291,4-Butanediol monovinyl etherHCID 637568Dimethyl Fumarate

생성물 1

HCID 86587517Bis(4-vinyloxybutyl) fumarate수율 95.2%

시약·촉매·용매 3

HCID 11192Zinc Acetate촉매HCID 64819Antioxidant 1010촉매HCID 887Methanol용매

실험 절차

Into a 1 L-volume flask equipped with a distillation unit, 144 g of dimethyl fumarate, 279 g of hydroxybutyl vinyl ether, 0.2 g of zinc acetate and 0.3 g of IRGANOX 1010 as a polymerization inhibitor were charged. The mixture was heated to 140° C. in a nitrogen atmosphere and methanol generated as a by-product was distilled off. When methanol reached 70% of the theoretical amount, the pressure inside of the reaction system was gradually reduced to accelerate the distillation of methanol, and by finally reducing the pressure to about 400 Pa, the theoretical amount of methanol and the residual hydroxybutyl vinyl ether were completely distilled off. The reaction solution was cooled to a room temperature and then 297 g of bis(4-vinyloxybutyl) fumarate was obtained.

후처리

  1. additionwere charged
  2. distillationwas distilled off
  3. distillationthe distillation of methanol
  4. distillationthe theoretical amount of methanol and the residual hydroxybutyl vinyl ether were completely distilled off

출처 및 근거

ORD 기록
ord-25717d553514433eb13306a17ff7ccc7
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07038076B2

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