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Methyl Acrylate → 3-[2,4,6-Tris(1-methylethyl)phenyl]-2-propenyl carboxylic acid, methyl ester

HRID 1781484
ノート
印刷プレビュー

反応式

HRID 1781484 の反応式
[C:1]([O:5][CH3:6])(=[O:4])[CH:2]=[CH2:3].[CH:7]([C:10]1[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[CH:13]=[C:12]([CH:19]([CH3:21])[CH3:20])[C:11]=1Br)([CH3:9])[CH3:8].[C:23](OCC)(=O)C>CN(C)C=O.C(N(CC)CC)C.[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH3:8][CH:7]([C:10]1[CH:15]=[C:14]([CH:16]([CH3:18])[CH3:17])[CH:13]=[C:12]([CH:19]([CH3:21])[CH3:20])[C:11]=1[CH:23]=[CH:3][CH2:2][C:1]([O:5][CH3:6])=[O:4])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 7294Methyl AcrylateHCID 8857Ethyl AcetateHCID 1408461-Bromo-2,4,6-triisopropylbenzene

生成物 1

HCID 867492493-[2,4,6-Tris(1-methylethyl)phenyl]-2-propenyl carboxylic acid, methyl ester

試薬・触媒・溶媒 3

HCID 6102075Dichlorobis(triphenylphosphine)palladium触媒
HCID 6228
Dimethylformamide
溶媒
HCID 8471Triethylamine溶媒

実験手順

A mixture of methyl acrylate (15.9 mL, 176 mmol) and bis (triphenylphosphine) palladium (II) chloride (0.99 g, 1.4 mmol) in 125 mL dimethylformamide and 125 mL triethylamine was heated to reflux for 1 hour and then 2,4,6 -triisopropylbromobenzene (10.0 g, 35 mmol) was added. Reflux was continued for 6 hours and then stirred at room temperature for 16 hours. Partitioned the reaction between water and diethyl ether. The ether layer was dried with MgSO4, filtered, and concentrated to give a brown oil. Chromatography (SiO2, eluant=5% ethyl acetate in hexanes) gave 3.80 g of 3-[2,4,6-tris(1-methylethyl)phenyl]-2-propenyl carboxylic acid, methyl ester as an off-white solid, mp 61°-63° C.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 1 hour
  3. temperatureReflux
  4. customPartitioned
  5. customthe reaction between water and diethyl ether
  6. dry with materialThe ether layer was dried with MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give a brown oil

出典と根拠

ORDレコード
ord-a415a2aa4c31427b970172b8ba449f65
出典データセット
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05633287

反応ノート

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