Fumaric Acid → Rosin fumaric acid

HRID 744857

反応式

HRID 744857 の反応式
[CH:1]1[CH:6]=[CH:5][C:4](/[CH:7]=[CH:8]/[CH2:9][O:10][C@@H:11]2[O:16][C@H:15]([CH2:17][OH:18])[C@@H:14]([OH:19])[C@H:13]([OH:20])[C@H:12]2[OH:21])=[CH:3][CH:2]=1.[C:22]([OH:29])(=[O:28])/[CH:23]=[CH:24]/[C:25]([OH:27])=[O:26]>>[CH:1]1[CH:2]=[CH:3][C:4](/[CH:7]=[CH:8]/[CH2:9][O:10][C@@H:11]2[O:16][C@H:15]([CH2:17][OH:18])[C@@H:14]([OH:19])[C@H:13]([OH:20])[C@H:12]2[OH:21])=[CH:5][CH:6]=1.[C:22]([OH:29])(=[O:28])/[CH:23]=[CH:24]/[C:25]([OH:27])=[O:26]

参加物

3

反応物 2

HCID 444972Fumaric AcidHCID 5280656(2R,3S,4S,5R,6R)-2-(hydroxymethyl)-6-[(E)-3-phenylprop-2-enoxy]oxane-3,4,5-triol3 回

生成物 1

HCID 131719576Rosin fumaric acid

実験手順

A resin was prepared according to the method of the present invention by placing 1000 grams of tall oil rosin in an autoclave equipped for heating, cooling, pressurizing and stirring the reaction medium. The rosin was heated to 200° C. under a nitrogen atmosphere. Fumaric acid in the amount of 210 grams was added to the heated rosin and the mixture was reacted for 2 hours at 200° C. at atmospheric pressure under a nitrogen gas blanket in order to form a rosin/fumaric acid adduct. At the end of the 2 hour reaction period, 270 grams of pentaerythritol were added to the rosin/fumaric acid adduct. The autoclave was sealed under nitrogen, and the temperature of the reaction mass was increased to 220° C. The pressure in the autoclave was allowed to build autogenously as the reaction progressed due to the formation of water during the esterification of the adduct. After approximately 4 hours, the reaction mixture had an acid number of about 145 (ASTM D465-59) and a softening point of 115° C. (ASTM E28-67). At this point, the pressure in the autoclave was about 75 psig (618 kPa). The reaction mass was then cooled to 185° C. and a mixture of 25 grams of dimethylethanolamine and 350 grams of water were pumped into the autoclave under pressure. As the water/amine solution was charged to the autoclave, the reaction mass was cooled to 130° C. At a temperature of 130° C., 225 grams of monoethanolamine were pumped into the autoclave. The reaction mass in the autoclave was cooled to a final temperature of 70° C. while charging the monoethanolamine. Final product analyses indicated that the product had a pH of 8.0 to 8.45, a solids content of 80 to 85 wt. % and a solution color of 16.

後処理

  1. customA resin was prepared
  2. customequipped
  3. temperaturefor heating
  4. temperaturecooling
  5. customthe mixture was reacted for 2 hours at 200° C. at atmospheric pressure under a nitrogen gas blanket in order

出典と根拠

ORDレコード
ord-a3b7e696b3854f2399849257eba1afc0
出典データセット
uspto-grants-1996_09
特許番号
US05559206

関連ノート

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