Methyl Methacrylate → 4-Phenylbutyl methacrylate

HRID 732157

반응식

HRID 732157 반응식
[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]

참가 물질

5

반응물 3

HCID 6658Methyl Methacrylate2회HCID 7638MonobenzoneHCID 3479713-Benzyloxy-1-propanol

생성물 1

HCID 225074774-Phenylbutyl methacrylate수율 213.7%

시약·촉매·용매 1

HCID 21801Titanium tetrabutoxide촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-175cdeb2f9c241f79475522c92a05037
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585900B2

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