Acrylic Acid → p-Butoxystyrene t-butyl acrylate acrylic acid

HRID 962374

反応式

HRID 962374 の反応式
[CH2:1]([O:5][C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[CH2:11])=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4].[C:14]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])(=[O:17])[CH:15]=[CH2:16].[C:23]([OH:27])(=[O:26])[CH:24]=[CH2:25].C(OOC(CC)(CCCC)C([O-])=O)(C)(C)C>CC(C)=O>[CH2:1]([O:5][C:6]1[CH:7]=[CH:8][C:9]([CH:10]=[CH2:11])=[CH:12][CH:13]=1)[CH2:2][CH2:3][CH3:4].[C:14]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])(=[O:17])[CH:15]=[CH2:16].[C:23]([OH:27])(=[O:26])[CH:24]=[CH2:25]

参加物

6

反応物 4

HCID 6581Acrylic AcidHCID 15458tert-Butyl acrylateHCID 11715272p-ButoxystyreneHCID 22065482t-Butylperoxy(2-ethylhexanoate)

生成物 1

HCID 86752681p-Butoxystyrene t-butyl acrylate acrylic acid収率 64%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
90 °C

実験手順

In an autoclave equipped with a 1.0-liter glass polymerization vessel and purged with nitrogen, polymerization reaction was carried out by dissolving 19.4 grams (0.11 mol) of p-butoxystyrene, 25.0 grams (0.20 mol) of t-butyl acrylate and 0.7 grams (0.01 mol) of acrylic acid in 300 grams of acetone, adding 3.5 grams of t-butylperoxy(2-ethylhexanoate) as a polymerization catalyst, and heating the mixture at 90° C. Thereafter, the catalyst was added in incremental amounts, that is, 1.0 grams after 21/2 hours and 1.0 grams after 41/2 hours from the start of polymerization reaction. After 6 hours of polymerization, the reaction solution was cooled down and the acetone was distilled off. A 9/1 methanol/water mixture was added to the reaction solution, causing the copolymer to crystallize. The copolymer had a weight average molecular weight (Mw) of 6,000, a dispersity (Mw/Mn) of 1.70, and a copolymerization ratio (p-butoxystyrene/t-butyl acrylate/acrylic acid) of 1:2:0.1. the yield was 64.0%.

後処理

  1. custompurged with nitrogen, polymerization reaction
  2. additionThereafter, the catalyst was added in incremental amounts
  3. custom1.0 grams after 21/2 hours and 1.0 grams after 41/2 hours from the start of polymerization reaction
  4. customAfter 6 hours of polymerization
  5. temperaturethe reaction solution was cooled down
  6. distillationthe acetone was distilled off
  7. additionA 9/1 methanol/water mixture was added to the reaction solution
  8. customto crystallize

出典と根拠

ORDレコード
ord-6335f9d163fd4bf880d354f486ab7e91
出典データセット
uspto-grants-1998_06
特許番号
US05759739

関連ノート

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