Dimethyl Fumarate → Tetramethyl cyclobutane-1,2,3,4-tetracarboxylatato(2-)

HRID 749624

反応式

HRID 749624 の反応式
[C:1]([O:9][CH3:10])(=[O:8])/[CH:2]=[CH:3]/[C:4]([O:6][CH3:7])=[O:5]>O>[CH:2]1([C:1]([O:9][CH3:10])=[O:8])[CH:3]([C:4]([O:6][CH3:7])=[O:5])[CH:2]([C:1]([O:9][CH3:10])=[O:8])[CH:3]1[C:4]([O:6][CH3:7])=[O:5]

参加物

3

反応物 1

HCID 637568Dimethyl Fumarate

生成物 1

HCID 266035Tetramethyl cyclobutane-1,2,3,4-tetracarboxylatato(2-)収率 100%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The dimethyl fumarate (1224 g, 8.5 mol) and water (4000 ml) were added to a 6-liter flask and irradiated by 365 nm ultraviolet lights at a temperature from 5 to 7° C. for 7 hours. The resultant solid in the flask was vacuum filtered to obtain tetramethyl cyclobutane-1,2,3,4-tetracarboxylate (1224 g, 4.25 mol). According to the NMR spectrum as shown in FIG. 1, dimethyl fumarate was present before the cyclization reaction. It can be observed from FIG. 2 that, after the cyclization reaction, the absorption peak at 6.77 ppm disappeared which means that dimethyl fumarate had been reacted completely. The absorption peak at 3.68 ppm represents the generation of the corresponding cyclobutanetetracarboxylate. FIGS. 1 and 2 prove that the yield of the reaction is almost 100%.

後処理

  1. customirradiated by 365 nm ultraviolet lights at a temperature from 5 to 7° C. for 7 hours
  2. filtrationfiltered

出典と根拠

ORDレコード
ord-f40ef0cbe9bd4178bc07ea3448a2523f
出典データセット
uspto-grants-2008_07
特許番号
US07402693B2

関連ノート

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