Triethylamine → HCID 20426788、化合物

HRID 434397

反応式

HRID 434397 の反応式
[CH3:1][Si:2]([CH3:11])([CH3:10])[C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:19](Cl)(=[O:22])[CH:20]=[CH2:21]>C1(C)C=CC=CC=1.C1(C=CC(O)=CC=1)O>[C:19]([O:9][C:6]1[CH:7]=[CH:8][C:3]([Si:2]([CH3:11])([CH3:10])[CH3:1])=[CH:4][CH:5]=1)(=[O:22])[CH:20]=[CH2:21]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 257324-(Trimethylsilyl)phenol

生成物 1

HCID 20426788HCID 20426788、化合物収率 83.5%

試薬・触媒・溶媒 2

HCID 785Hydroquinone触媒HCID 1140Toluene溶媒

実験手順

8.32 g (0.05 mole) of p-trimethylsilylphenol was dissolved in 25 ml toluene. 6.1 g (0.06 mole) triethyl amine and 0.05 g hydroquinone was added. The solution was warmed. 5.43 g (0.06 mole) of acryloyl chloride was added over a 15 minute period. After 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water and separated. After washing with brine and separating, the organic phase was dried over magnesium sulfate, filtered, and the solvent removed in a rotary evaporator under reduced pressure. Vacuum distillation yielded 9.2 g of pure p-trimethylsilylphenyl acrylate.

後処理

  1. temperatureThe solution was warmed
  2. washAfter 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water
  3. customseparated
  4. washAfter washing with brine
  5. customseparating
  6. dry with materialthe organic phase was dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent removed in a rotary evaporator under reduced pressure
  9. distillationVacuum distillation

出典と根拠

ORDレコード
ord-0130afa88989486ea49d5a69d9c4a3f1
出典データセット
uspto-grants-1983_08
特許番号
US04396704

関連ノート

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