Methacrylic Acid → Methyl methacrylate methoxyethyl methacrylate benzyl methacrylate methacrylic acid

HRID 2389203

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HRID 2389203 반응식
[C:1]([O:6][CH3:7])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:8]([O:12][CH2:13][CH2:14][O:15][CH3:16])(=[O:11])[CH:9]=[CH2:10].[C:17]([O:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)(=[O:21])[C:18]([CH3:20])=[CH2:19].[C:30]([OH:35])(=[O:34])[C:31]([CH3:33])=[CH2:32].N(C(C)(C)C(OC)=O)=NC(C)(C)C(OC)=O>C(O)(C)C.C(C(C)=O)C>[C:1]([O:6][CH3:7])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:8]([O:12][CH2:13][CH2:14][O:15][CH3:16])(=[O:11])[C:9]([CH3:17])=[CH2:10].[C:17]([O:22][CH2:23][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1)(=[O:21])[C:18]([CH3:20])=[CH2:19].[C:30]([OH:35])(=[O:34])[C:31]([CH3:33])=[CH2:32]

참가 물질

8

반응물 5

HCID 4093Methacrylic AcidHCID 6658Methyl MethacrylateHCID 17236Benzyl methacrylateHCID 183922-Methoxyethyl acrylateHCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)3회

생성물 1

HCID 131729954Methyl methacrylate methoxyethyl methacrylate benzyl methacrylate methacrylic acid

시약·촉매·용매 2

HCID 3776Isopropanol용매HCID 6569Methyl Ethyl Ketone용매3회

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온도
87 °C

실험 절차

560.0 g of methyl ethyl ketone was placed in a 2 L three-necked flask equipped with a stirrer, a thermometer, and a reflux cooling tube, and heated to a temperature of 87° C. While maintaining the gas inside the reaction vessel in a refluxed state (thereafter, refluxing was continued until the reaction was completed), to this reaction vessel, a mixture including 266.8 g of methyl methacrylate, 63.8 g of methoxyethyl acrylate, 203 g of benzyl methacrylate, 46.4 g of methacrylic acid, and 2.32 g of “V-601” (trade name, manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise at a constant speed so as to complete the addition in two hours. After completing the addition, the resulting mixture was stirred for one hour. Thereafter, a solution of 1.16 g of “V-601” and 6.4 g of methyl ethyl ketone was added thereto, and the mixture thus obtained was stirred for two hours (process (1)). Subsequently, this process (1) was repeated for four times. Then, a solution of 1.16 g of “V-601” and 6.4 g of methyl ethyl ketone was further added, and stirring was continued for 3 hours. After completion of the polymerization reaction, the temperature of the resulting solution was lowered to 65° C. and then, 163.0 g of isopropanol was added thereto and cooled while leaving it standing still. In this way, a resin solution of a copolymer (methyl methacrylate/methoxyethyl methacrylate/benzyl methacrylate/methacrylic acid=46/11/35/8) was obtained. The obtained copolymer had a weight average molecular weight (Mw) of 63,000 and an acid value of 65.1 mgKOH/g.

후처리

  1. customequipped with a stirrer
  2. temperaturea thermometer, and a reflux cooling tube
  3. temperatureWhile maintaining the gas inside the reaction vessel in a refluxed state (thereafter,
  4. temperaturerefluxing
  5. additionwas added dropwise at a constant speed so as
  6. additionthe addition in two hours
  7. additionthe addition
  8. customthe mixture thus obtained
  9. stirringstirring
  10. waitwas continued for 3 hours
  11. customAfter completion of the polymerization reaction
  12. customwas lowered to 65° C.
  13. temperaturecooled
  14. customwhile leaving it

출처 및 근거

ORD 기록
ord-38cfde75e10940888fd5bbee389c6308
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08272732B2

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