Diethylene Glycol → Diethylene glycol monoacrylate

HRID 1044447노트

반응식

HRID 1044447 반응식
[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]

참가 물질

5

반응물 3

HCID 8117Diethylene GlycolHCID 8471TriethylamineHCID 13140Acryloyl chloride

생성물 1

HCID 61642Diethylene glycol monoacrylate수율 48.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dcde9ba500b245bd84a94ef36d9c6816
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563624B2

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