4-Chloroquinazoline → Ethyl 1-quinazolin-4-ylindolin-3-ylacetate

HRID 597041ノート

反応式

HRID 597041 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][N:3]=1.[NH:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]([CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:13]1>COCCOC>[N:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:2]([N:12]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[CH:14]([CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:13]2)=[N:3][CH:4]=1

参加物

4

反応物 2

HCID 788644-ChloroquinazolineHCID 21795444Ethyl (2,3-dihydro-1H-indol-3-yl)acetate

生成物 1

HCID 54457736Ethyl 1-quinazolin-4-ylindolin-3-ylacetate

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

A mixture of 4-chloroquinazoline (2.3g.) and ethyl indolin-3-ylacetate (2.6g.) in 1,2-dimethoxyethane (30ml.) was heated under reflux for 15 minutes. The mixture was cooled and filtered, and the solid residue was dissolved in ice-water (40ml.). To the solution was added saturated sodium acetate solution (10ml.), and the mixture was extracted with ethyl acetate (3 × 50ml.). The combined extracts were dried (Na2SO4), and the solvent evaporated in vacuo to give ethyl 1-quinazolin-4-ylindolin-3-ylacetate as a syrup which was proved to be pure by TLC (system A).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 15 minutes
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. dissolutionthe solid residue was dissolved in ice-water (40ml.)
  6. additionTo the solution was added saturated sodium acetate solution (10ml.)
  7. extractionthe mixture was extracted with ethyl acetate (3 × 50ml.)
  8. dry with materialThe combined extracts were dried (Na2SO4)
  9. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-dcde0069e29d44d29c10c2b03b9f218d
出典データセット
uspto-grants-1977_03
特許番号
US04012513

反応ノート

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