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Sulfur → 1-(Cyclopropylmethyl)-6-methoxy-4-phenyl-2(1H)-quinazolinone

HRID 2166558
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반응식

HRID 2166558 반응식
[CH:1]1([CH2:4][N:5]2[C:14]3[C:9](=[CH:10][C:11]([O:15][CH3:16])=[CH:12][CH:13]=3)[CH:8]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[NH:7][C:6]2=[O:23])[CH2:3][CH2:2]1.[S]>ClC1C=CC=CC=1Cl>[CH:1]1([CH2:4][N:5]2[C:14]3[C:9](=[CH:10][C:11]([O:15][CH3:16])=[CH:12][CH:13]=3)[C:8]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)=[N:7][C:6]2=[O:23])[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 5362487SulfurHCID 131890501-cyclopropylmethyl-4-phenyl-6-methoxy-3,4-dihydro-2(1H)-quinazolinone

생성물 1

HCID 364891-(Cyclopropylmethyl)-6-methoxy-4-phenyl-2(1H)-quinazolinone수율 88.2%

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

실험 절차

A mixture of 1.54 g of 1-cyclopropylmethyl-4-phenyl-6-methoxy-3,4-dihydro-2(1H)-quinazolinone, 0.48 g of sulfur and 10 ml of o-dichlorobenzene was stirred under reflux for 5 hours. The solvent was then removed under reduced pressure, and the residue was treated with hot acetone. The insoluble sulfur was filtered off and the filtrate was concentrated to dryness. The residue was recrystallized from toluene to give 1.35 g of 1-cyclopropylmethyl-4-phenyl-6-methoxy-2(1H)-quinazolinone, m.p. 114°-115° C.

후처리

  1. temperatureunder reflux for 5 hours
  2. customThe solvent was then removed under reduced pressure
  3. additionthe residue was treated with hot acetone
  4. filtrationThe insoluble sulfur was filtered off
  5. concentrationthe filtrate was concentrated to dryness
  6. customThe residue was recrystallized from toluene

출처 및 근거

ORD 기록
ord-2643f18b3a3247edb13b4389eee9b889
출처 데이터셋
uspto-grants-1983_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04387223

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