Methyl Methacrylate → Isodecyl methacrylate

HRID 2248069

反応式

HRID 2248069 の反応式
[CH2:1]([OH:11])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]([CH3:10])[CH3:9].[C:12](OC)(=[O:16])[C:13]([CH3:15])=[CH2:14].C(N(CC)O)C.C1C2NC3C(=CC=CC=3)SC=2C=CC=1>>[C:12]([O:11][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]([CH3:9])[CH3:10])(=[O:16])[C:13]([CH3:15])=[CH2:14]

参加物

5

反応物 4

HCID 6658Methyl MethacrylateHCID 7108PhenothiazineHCID 19463DiethylhydroxylamineHCID 32898Isodecanol2 回

生成物 1

HCID 34763Isodecyl methacrylate収率 99%

実験手順

Four hundred seventy four grams (3.0 moles) of isodecyl alcohol, 750 g (7.5 moles) of methyl methacrylate (MMA), 1.75 g (3.0 millimol) of hafnium actylacetonate, and 50 mg diethylhydroxylamine and 25 mg phenothiazine free radical polymerization inhibitors, are added to a 3 liter flask equipped with an agitator, thermometer, and a 10-plate Oldershaw fractional distillation column. The mixture was heated to reflux at atmospheric pressure while an azeotropic mixture of MMA and methanol was removed from the upper part of the fractionating column. The reaction was continued in this manner for approximately 90 minutes while the temperature at the top of the column was 65°-67° C. and the temperature in the pot was 106°-124° C. Excess MMA was removed under vacuum and the resulting IDMA was isolated (660 grams, 99.0% yield) and analyzed. Gas-liquid chromatographic (GLC) analysis showed >99.9% conversion of isodecanol to IDMA of 99.8% purity.

後処理

  1. additionare added to a 3 liter flask
  2. customequipped with an agitator
  3. distillationthermometer, and a 10-plate Oldershaw fractional distillation column
  4. temperatureThe mixture was heated
  5. temperatureto reflux at atmospheric pressure while an azeotropic mixture of MMA and methanol
  6. customwas removed from the upper part of the fractionating column
  7. customwas 65°-67° C.
  8. custompot was 106°-124° C
  9. customExcess MMA was removed under vacuum
  10. customthe resulting IDMA was isolated (660 grams, 99.0% yield)

出典と根拠

ORDレコード
ord-695ae2277df447a99afb5b1ca4563d53
出典データセット
uspto-grants-1991_08
特許番号
US05037978

関連ノート

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