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Methyl Methacrylate → Propylene glycol methyl ether acetate

HRID 627813
ノート
印刷プレビュー

反応式

HRID 627813 の反応式
C[Si](O[C:6]([O:10][CH3:11])=[C:7](C)[CH3:8])(C)C.ClC1C=[C:15](C=CC=1)[C:16]([O-:18])=[O:17].C([N+](CCCC)(CCCC)CCCC)CCC.C(OC)(=O)C(C)=C.C(OCCN(C)C)(=O)C(C)=C>CO.C(#N)C.O1CCCC1>[C:16]([O:18][CH:7]([CH3:8])[CH2:6][O:10][CH3:11])(=[O:17])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6658Methyl MethacrylateHCID 17869(Dimethylamino)ethyl methacrylateHCID 552336Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl-HCID 21922187Tetrabutylammonium m-chlorobenzoate

生成物 1

HCID 7946Propylene glycol methyl ether acetate

試薬・触媒・溶媒 3

HCID 887
Methanol
溶媒
HCID 6342Acetonitrile溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

A 500 mL four-necked round-bottom separable flask was equipped with a condenser tube, a dropping funnel, a nitrogen inlet, a stirrer and a thermometer. Tetrahydrofuran (THF) of 250 parts by weight and dimethylketene methyl trimethylsilyl acetal of 2.32 parts by weight, which is an initiator, were poured into the flask through the dropping funnel, followed by sufficient nitrogen substitution. Then, 0.2 part by weight of 1 mol/L acetonitrile solution of tetrabutylammonium m-chlorobenzoate, which is a catalyst, was injected with a syringe. Methyl methacrylate (hereinafter may be referred to as MMA) of 93.3 parts by weight was added dropwise with the dropping funnel for 60 minutes. While cooling the separable flask, the temperature was kept below 40° C. One hour later, dimethylaminoethyl methacrylate (hereinafter may be referred to as DMMA) of 40.0 parts by weight was added dropwise for 20 minutes. After one hour reaction, methanol of 0.5 parts by mass was added to terminate the reaction. The thus-obtained copolymer THF solution was reprecipitated in hexane, filtrated, dried in vacuum and then purified, thus obtaining a polymer. To the amine-containing polymer obtained in this manner of 60 parts by weight, propylene glycol monomethyl ether acetate (hereinafter may be referred to as PGMEA) of 40 parts by weight was added and uniformly mixed to obtain a polymer solution B1. For the polymer solution B1, GPC was measured with HLC-8220 equipped with an RI detector (manufactured by Tosoh Corporation), using THF as the developing solvent and a molecular weight standard polymer as the standard polystyrene, thus obtaining the molecular weight distribution and mass average molecular weight. The amine value was 115 mg KOH/g. The mass average molecular weight Mw was 9,900. The number average molecular weight Mn was 8,320. The molecular weight distribution Mw/Mn was 1.19 (MMA/DMMA mass ratio: 7/3).

後処理

  1. customA 500 mL four-necked round-bottom separable flask was equipped with a condenser tube, a dropping funnel, a nitrogen inlet, a stirrer
  2. additionwere poured into the flask through the dropping funnel
  3. customwas injected with a syringe
  4. temperatureWhile cooling the separable flask
  5. customwas kept below 40° C
  6. additionwas added
  7. customto terminate
  8. customthe reaction
  9. customThe thus-obtained copolymer THF solution was reprecipitated in hexane
  10. filtrationfiltrated
  11. customdried in vacuum
  12. custompurified
  13. customthus obtaining a polymer

出典と根拠

ORDレコード
ord-5d2144f3b41b405c96f4667a0583cd0a
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309399B2

反応ノート

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