Ethylene Glycol → HCID 66596793, 화합물

HRID 503992노트

반응식

HRID 503992 반응식
[CH3:1][O:2][C:3]1[C:12]2[NH:11][C:10](=[O:13])[CH2:9][CH2:8][C:7]=2[C:6]([CH:14]=[O:15])=[CH:5][CH:4]=1.[CH2:16](O)[CH2:17][OH:18].C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[O:15]1[CH2:16][CH2:17][O:18][CH:14]1[C:6]1[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[C:12]2[C:7]=1[CH2:8][CH2:9][C:10](=[O:13])[NH:11]2

참가 물질

6

반응물 3

HCID 174Ethylene GlycolHCID 516892Sodium BicarbonateHCID 859802658-Methoxy-2-oxo-1,2,3,4-tetrahydroquinoline-5-carboxaldehyde

생성물 1

HCID 66596793HCID 66596793, 화합물수율 70%

시약·촉매·용매 2

HCID 521998p-Toluenesulfonic acid monohydrate촉매HCID 1140Toluene용매

실험 절차

8-Methoxy-2-oxo-1,2,3,4-tetrahydroquinoline-5-carboxaldehyde (42 g) was suspended in toluene (400 ml), and ethylene glycol (33.7 ml) and p-toluenesulfonic acid monohydrate (0.78 g) were added, and the resulting mixture was heated under reflux in a Dean-Stark apparatus for 4.5 hours. The reaction mixture was cooled, and 10 ml of an aqueous solution containing 1.72 g of sodium bicarbonate was added. Stirring was carried out for some time, and the produced solid was collected by filtration. The solid was washed with water and toluene and dried at 60° C. to thereby obtain 35.5 g (yield: 70%) of 5-(1,3-dioxolan-2-yl)-8-methoxy-3,4-dihydro-1H-quinolin-2-one as white crystals.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux in a Dean-Stark apparatus for 4.5 hours
  3. temperatureThe reaction mixture was cooled
  4. additionwas added
  5. filtrationthe produced solid was collected by filtration
  6. washThe solid was washed with water and toluene
  7. customdried at 60° C.

출처 및 근거

ORD 기록
ord-1e2553d19e084690b34f86c8bec65b9a
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07777038B2

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