Methyl Methacrylate → 4-Phenylbutyl methacrylate

HRID 480990

反応式

HRID 480990 の反応式
[C:1]([O:6][CH3:7])(=[O:5])[C:2]([CH3:4])=[CH2:3].[CH2:8](OCCCO)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[CH2:20](OC1C=CC(O)=CC=1)[C:21]1C=CC=CC=1>[O-]CCCC.[O-]CCCC.[O-]CCCC.[O-]CCCC.[Ti+4]>[C:1]([O:6][CH2:7][CH2:20][CH2:21][CH2:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)(=[O:5])[C:2]([CH3:4])=[CH2:3]

参加物

5

反応物 3

HCID 6658Methyl Methacrylate2 回HCID 7638MonobenzoneHCID 3479713-Benzyloxy-1-propanol

生成物 1

HCID 225074774-Phenylbutyl methacrylate収率 213.7%

試薬・触媒・溶媒 1

HCID 21801Titanium tetrabutoxide触媒

実験手順

A three neck round bottom flask containing a teflon coated magnetic stirring bar was successively charged with 95 mL (0.884 mol) of methyl methacrylate (2), 4.22 g (0.012 mol) of titanium tetrabutoxide (Ti(OC4H9)4), 50 mL (0.316 mol) of 3-benzyloxy-1-propanol (1), and 14.6 g (0.073 mol) of 4-benzyloxyphenol (4-BOP). An addition funnel, thermometer, and a short path still head with thermometer and receiver flask were placed in the flask necks. The flask was placed in an oil bath and the temperature was increased until distillation began. Methyl methacrylate (2) was placed in the addition funnel and was added dropwise at the same rate as the distillate. The reaction mixture was heated for 4 hours and then cooled to room temperature. The crude product was vacuum distilled to isolate 36.5 g (0.156 mol, 49%) of 3-benzyloxypropyl methacrylate (3) as a clear, colorless liquid.

後処理

  1. additionA three neck round bottom flask containing a teflon coated magnetic stirring bar
  2. customAn addition funnel, thermometer, and a short path still head with thermometer and receiver flask were placed in the flask necks
  3. customThe flask was placed in an oil bath
  4. temperaturethe temperature was increased until distillation
  5. additionwas added dropwise at the same rate as the distillate
  6. temperatureThe reaction mixture was heated for 4 hours
  7. distillationdistilled

出典と根拠

ORDレコード
ord-c745c41559344da384c7120717f66ec7
出典データセット
uspto-grants-2003_11
特許番号
US06653422B2

関連ノート

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