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Methyl Methacrylate → 4-Phenylbutyl methacrylate

HRID 480989
ノート
印刷プレビュー

反応式

HRID 480989 の反応式
[C:1]([O:6][CH3:7])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:8]1([CH2:14][CH2:15][CH2:16]CO)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(OC1C=CC(O)=CC=1)C1C=CC=CC=1>[O-]CCCC.[O-]CCCC.[O-]CCCC.[O-]CCCC.[Ti+4]>[C:1]([O:6][CH2:7][CH2:16][CH2:15][CH2:14][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)(=[O:5])[C:2]([CH3:4])=[CH2:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6658Methyl Methacrylate2 回HCID 7638MonobenzoneHCID 76889Benzenebutanol

生成物 1

HCID 225074774-Phenylbutyl methacrylate収率 74.4%

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 120 mL (1.09 mol) of methyl methacrylate (2), 5.35 g (0.015 mol) of titanium tetrabutoxide (Ti(OC4H9)4), 60 mL (0.39 mol) of 4-phenyl-1-butanol (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 62.8 g (0.29 mol, 74%) of 4-phenylbutyl methacrylate (3) as a clear, colorless liquid. Example 2: Synthesis of 3-benzyloxypropyl methacrylate.

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-09bad5a9cd8c487ba14ee78c83cf96c4
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06653422B2

反応ノート

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