Methyl Methacrylate → Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

HRID 35152

反応式

HRID 35152 の反応式
[C:1]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])(=[O:4])[CH:2]=[CH2:3].[C:10]([O:15][CH3:16])(=[O:14])[C:11]([CH3:13])=[CH2:12].C(=O)([O-])[O-].[Na+].[Na+]>O.[N+]([O-])(O)=O>[C:1]([O:5][CH2:6][CH2:7][CH2:8][CH3:9])(=[O:4])[CH:2]=[CH2:3].[C:10]([O:15][CH3:16])(=[O:14])[C:11]([CH3:13])=[CH2:12]

参加物

6

反応物 3

HCID 6658Methyl MethacrylateHCID 8846Butyl AcrylateHCID 10340Sodium Carbonate

生成物 1

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

試薬・触媒・溶媒 2

HCID 944Nitric Acid溶媒HCID 962Water溶媒

実験手順

Cellulose (200 g, Harmac fully bleached Douglas Fir pulp available from MacMillan Bloedel, Stamford, CT) was dispersed in water (9.5 l) by mechanical agitation under nitrogen purging for two hours. A mixture of butyl acrylate (200 g) and methyl methacrylate (20 g) was vigorously stirred into the pulp for one-half hour. Graft copolymerization was initiated by addition of ceric ammonium nitrate (11 g, 0.02M) in 1M nitric acid (500 ml). The graft copolymerization was allowed to proceed for four hours, during which the color of the aqueous portion went from yellow (Ce4) to colorless (Ce3) indicating the oxidation of cellulose and initiation of polymerization. The reaction was neutralized with sodium carbonate (26.5 g, 0.25 M), filtered by suction, and washed with water (5 l). The sample was dried overnight at 90° C. to give a white fiber product (405 g, 93% conversion). The cellulose graft copolymer was extracted by refluxing with tetrahydrofuran (9 l) for three hours to remove homopolymer, filtered and dried to yield cellulose/butyl acrylate/methyl methacrylate fibers (200 g/177 g, 53 wt. % cellulose/47 wt. % butyl acrylate/methyl methacrylate, 86% graft efficiency).

後処理

  1. customGraft copolymerization
  2. customThe graft copolymerization
  3. filtrationfiltered by suction
  4. washwashed with water (5 l)
  5. customThe sample was dried overnight at 90° C.
  6. customto give a white fiber product (405 g, 93% conversion)
  7. extractionThe cellulose graft copolymer was extracted
  8. temperatureby refluxing with tetrahydrofuran (9 l) for three hours
  9. customto remove homopolymer
  10. filtrationfiltered
  11. customdried

出典と根拠

ORDレコード
ord-2548f1f26ad649c8805369e662cb133a
出典データセット
uspto-grants-1988_08
特許番号
US04765982

関連ノート

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