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

HRID 1823641

反応式

HRID 1823641 の反応式
[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]

参加物

6

反応物 2

HCID 873291,4-Butanediol monovinyl etherHCID 637568Dimethyl Fumarate

生成物 1

HCID 86587517Bis(4-vinyloxybutyl) fumarate収率 95.2%

試薬・触媒・溶媒 3

HCID 11192Zinc Acetate触媒HCID 64819Antioxidant 1010触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-25717d553514433eb13306a17ff7ccc7
出典データセット
uspto-grants-2006_05
特許番号
US07038076B2

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