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Ethylene Glycol → HCID 19600975, 화합물

HRID 610079
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HRID 610079 반응식
[C:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[N:9]([CH2:13][C:14]([F:17])([F:16])[F:15])[C:8](=[O:18])[CH2:7]2)(=[O:3])[CH3:2].[CH2:19](O)[CH2:20][OH:21].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1.C(OCC)(=O)C>[CH3:2][C:1]1([C:4]2[CH:5]=[C:6]3[C:10](=[CH:11][CH:12]=2)[N:9]([CH2:13][C:14]([F:15])([F:16])[F:17])[C:8](=[O:18])[CH2:7]3)[O:21][CH2:20][CH2:19][O:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 19600991HCID 19600991, 화합물

생성물 1

HCID 19600975HCID 19600975, 화합물

시약·촉매·용매 2

HCID 241Benzene용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 5-acetyl-1-(2,2,2-trifluoro-ethyl)-1,3-dihydro-indol-2-one (1.04 g, 4.0 mmol), ethylene glycol (1.37 mL, 24 mmol) and p-toluenesulfonic acid (10 mg) in benzene (25 mL) was heated to reflux for 4 hours in a flask fitted with a Dean-Stark trap. The solution was diluted with ethyl acetate, washed with saturated sodium bicarbonate, water and brine, dried over magnesium sulfate and concentrated in vacuo to an oil which solidified upon standing (1.19 g, 98%, mp 87-89° C.).

후처리

  1. temperatureto reflux for 4 hours in a flask
  2. customfitted with a Dean-Stark trap
  3. washwashed with saturated sodium bicarbonate, water and brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo to an oil which

출처 및 근거

ORD 기록
ord-ae4230352a1e4ad38e40a135d620c34e
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998463

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