Diethylene Glycol → Diethylene glycol monoacrylate

HRID 1483862ノート

反応式

HRID 1483862 の反応式
[CH2:1]([OH:7])[CH2:2][O:3][CH2:4][CH2:5][OH:6].C(N(CC)CC)C.[C:15](Cl)(=[O:18])[CH:16]=[CH2:17]>C1COCC1>[C:15]([O:7][CH2:1][CH2:2][O:3][CH2:4][CH2:5][OH:6])(=[O:18])[CH:16]=[CH2:17]

参加物

5

反応物 3

HCID 8117Diethylene GlycolHCID 8471TriethylamineHCID 13140Acryloyl chloride

生成物 1

HCID 61642Diethylene glycol monoacrylate収率 48.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

25 g (0.235 mol) of diethylene glycol was dissolved in 150 mL of THF. 18 mL of (0.13 mol) of triethyl amine was added, followed by the dropwise addition of 10.8 g (8 mL, 0.12 mol) of acryloyl chloride. The reaction temperature was kept below 30° C. The reaction was allowed to continue for 2 hours at room temperature. The precipitated triethyl amine hydrochloride was removed by filtration, 100 mg BHT was added and the solvent was removed under reduced pressure. Diethylene glycol monoacrylate was purified on a Prochrom LC80-system, using Kromasil 60A 10 μm spherical silica. Methylene chloride/ethyl acetate 60/40 was used as eluent at a flow rate of 200 mL/min. 10 mg BHT was added before evaporation of the eluent. 9.4 g of diethylene glycol monoacrylate was isolated.

後処理

  1. customwas kept below 30° C
  2. customThe precipitated triethyl amine hydrochloride was removed by filtration, 100 mg BHT
  3. additionwas added
  4. customthe solvent was removed under reduced pressure
  5. customDiethylene glycol monoacrylate was purified on a Prochrom LC80-system
  6. addition10 mg BHT was added before evaporation of the eluent

出典と根拠

ORDレコード
ord-71236422a0ff44219d9270e9264889b6
出典データセット
uspto-grants-2016_08
特許番号
US09416287B2

反応ノート

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