Sodium Hydroxide → 10-Benzyl-2,3-dihydroimidazo(2,1-B)quinazolin-5(10H)-one

HRID 918188

반응식

HRID 918188 반응식
[CH2:1]([N:8]1[C:14](=O)[O:13][C:11](=O)[C:10]2=[CH:16][CH:17]=[CH:18][CH:19]=[C:9]12)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CSC1[NH:23][CH2:24][CH2:25][N:26]=1.[OH-].[Na+]>O1CCOCC1>[CH2:1]([N:8]1[C:9]2[C:10](=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:11](=[O:13])[N:23]2[CH2:24][CH2:25][N:26]=[C:14]12)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 883692-Methylthio-2-imidazoline hydroiodideHCID 520756N-Benzylisatoic anhydride

생성물 1

HCID 413451510-Benzyl-2,3-dihydroimidazo(2,1-B)quinazolin-5(10H)-one

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 12.7 g. of N-benzylisatoic anhydride, 5.8 g. of 2-methylmercapto-imidazoline and 2 pellets of sodium hydroxide in 200 ml. of dioxane was refluxed for 2 hours. While still hot, the mixture was then filtered through Celite and the filtrate concentrated to about 50 ml. volume. 50 ml. of diethyl ether was added and the crystalline precipitate removed by filtration. The residue was dissolved in methylene chloride, treated with charcoal, filtered through alumina, and the filtrate evaporated. The residue was crystallized from methylene chloride/diethyl ether to obtain the heading compound, m.p. 203°-205°C.

후처리

  1. additionA mixture of 12.7 g
  2. filtrationWhile still hot, the mixture was then filtered through Celite
  3. concentrationthe filtrate concentrated to about 50 ml
  4. additionof diethyl ether was added
  5. customthe crystalline precipitate removed by filtration
  6. dissolutionThe residue was dissolved in methylene chloride
  7. additiontreated with charcoal
  8. filtrationfiltered through alumina
  9. customthe filtrate evaporated
  10. customThe residue was crystallized from methylene chloride/diethyl ether
  11. customto obtain the heading compound, m.p. 203°-205°C.

출처 및 근거

ORD 기록
ord-13f84b6891f14562918c92aaa3ad36b8
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03969506

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