Sulfuric Acid → Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

HRID 1013617

反応式

HRID 1013617 の反応式
S(=O)(=O)(O)O.[C:6]([O:11][CH3:12])(=[O:10])[C:7]([CH3:9])=[CH2:8].[C:13]([O:17][CH2:18][CH2:19][CH2:20][CH3:21])(=[O:16])[CH:14]=[CH2:15].C(S)CCCCCCCCCCC>O>[C:6]([O:11][CH3:12])(=[O:10])[C:7]([CH3:9])=[CH2:8].[C:13]([O:17][CH2:18][CH2:19][CH2:20][CH3:21])(=[O:16])[CH:14]=[CH2:15]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 6658Methyl Methacrylate2 回HCID 81951-Dodecanethiol2 回HCID 8846Butyl Acrylate2 回

生成物 1

HCID 62802Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

5 parts of mercapto-terminated PVA (having an ethylene content of 0.5 mol %, a degree of polymerization of 550, a saponification degree of 88.3 mol % and a mercapto group content of 3.3×10−5 equivalent/g) (PVA-213) and 90 parts of ion-exchanged water were fed into a glass vessel equipped with a reflux condenser, a dropping funnel, a thermometer, a nitrogen inlet mouth and a stirrer, and completely dissolved at 95° C. Next, its pH was made to be 4 with diluted sulfuric acid added thereto, and then 10 parts of methyl methacrylate, 10 parts of n-butyl acrylate and 0.1 parts of n-dodecylmercaptan were added to it with stirring at 150 rpm. This was purged with nitrogen and heated up to 70° C. 5 parts of 1% potassium persulfate was added to it to start the polymerization. Then, a mixture of 40 parts of methyl methacrylate, 40 parts of n-butyl acrylate and 0.4 parts of n-dodecylmercaptan was continuously added to it, over a period of 2 hours. 3 hours after the start of the polymerization, the conversion reached 99.5%, and the polymerization was stopped in this stage. The process gave stable methyl methacrylate/n-butyl acrylate copolymer emulsion (Em-214) having a solid concentration of 52.0%.

後処理

  1. custom5 parts of mercapto-terminated PVA (
  2. customa degree of polymerization of 550
  3. customequipped with a reflux condenser, a dropping funnel
  4. dissolutiona thermometer, a nitrogen inlet mouth and a stirrer, and completely dissolved at 95° C
  5. additionadded
  6. customThis was purged with nitrogen
  7. addition5 parts of 1% potassium persulfate was added to it
  8. customthe polymerization
  9. additionwas continuously added to it, over a period of 2 hours
  10. custom3 hours after the start of the polymerization

出典と根拠

ORDレコード
ord-74bdc21e44394ce0830bdfedb6338fd8
出典データセット
uspto-grants-2011_07
特許番号
US07981958B1

関連ノート

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