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3-Bromo-1-phenylpropane-1,2-dione → (5-Methoxy-6,7,8,9-tetrahydroimidazo[1,2-a]quinazolin-2-yl)-phenylmethanone

HRID 371392
ノート
印刷プレビュー

反応式

HRID 371392 の反応式
[CH3:1][O:2][C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[N:6]=[C:5]([NH2:13])[N:4]=1.Br[CH2:15][C:16](=O)[C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:18]>CCOCC>[CH3:1][O:2][C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[N:6]2[CH:15]=[C:16]([C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:18])[N:13]=[C:5]2[N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 125689113-Bromo-1-phenylpropane-1,2-dioneHCID 133009284-Methoxy-5,6,7,8-tetrahydroquinazolin-2-amine

生成物 1

HCID 10402951(5-Methoxy-6,7,8,9-tetrahydroimidazo[1,2-a]quinazolin-2-yl)-phenylmethanone

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A solution of 20 g of 4-methoxy-5,6,7,8-tetrahydro-2-quinazolinamine, 28.6 g of 3-bromo-1-phenyl-propane- 1,2-dione and 400 ml of ether was stirred overnight at room temperature and was filtered. The 29.5 g of 4-methoxy-1-(3-phenyl-2,3-dioxopropyl)-5,6,7,8-tetrahydro-2-quinazolinium bromide were washed with ether and suspended in methanol. The suspension was refluxed for 2 hours and the solution was evaporated to dryness under reduced pressure. The residue was shaken with a mixture of aqueous potassium carbonate and chloroform and the decanted organic phase was washed with water, dried over magnesium sulfate and evaporated to dryness under reduced pressure. The residue was triturated with ethanol and filtered to obtain 18 g of (5-methoxy-6,7,8,9-tetrahydroimidazo[1,2-a]quinazolin-2-yl-phenylmethanone in the form of pale yellow crystals melting at 234° C.

後処理

  1. filtrationwas filtered
  2. washThe 29.5 g of 4-methoxy-1-(3-phenyl-2,3-dioxopropyl)-5,6,7,8-tetrahydro-2-quinazolinium bromide were washed with ether
  3. temperatureThe suspension was refluxed for 2 hours
  4. customthe solution was evaporated to dryness under reduced pressure
  5. washthe decanted organic phase was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated to dryness under reduced pressure
  8. customThe residue was triturated with ethanol
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-551ed0d5859446bcabfca810110c0562
出典データセット
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04532243

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート