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Water → 3-Phenyl-2-[(4-methylpyridin-2-yl)methylthio]-4(3H)-quinazolinone

HRID 1085065
ノート
印刷プレビュー

反応式

HRID 1085065 の反応式
C[O-].[Na+].[SH:4][C:5]1[N:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:13](=[O:21])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]=1.Cl.Cl[CH2:24][C:25]1[CH:30]=[C:29]([CH3:31])[CH:28]=[CH:27][N:26]=1.O>CO>[C:15]1([N:14]2[C:13](=[O:21])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[N:6]=[C:5]2[S:4][CH2:24][C:25]2[CH:30]=[C:29]([CH3:31])[CH:28]=[CH:27][N:26]=2)[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 10942334Sodium MethoxideHCID 200610712-(Chloromethyl)-4-methylpyridine hydrochlorideHCID 178515047HCID 178515047、化合物

生成物 1

HCID 145751693-Phenyl-2-[(4-methylpyridin-2-yl)methylthio]-4(3H)-quinazolinone収率 30.7%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

8.7 ml of 28% methanolic solution of sodium methoxide were added to a solution of 5.0 g of 2-mercapto-3-phenyl-4(3H)-quinazolinone and 4.0 g of 2-chloromethyl-4-methylpyridine hydrochloride in methanol, and the stirring was continued at room temperature for 5 hours. The reaction solution was poured into water and extracted with chloroform. The chloroform layer was washed with an aqueous solution of sodium carbonate and dried over sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography. The fraction eluted with 8% ethyl acetate in chloroform was collected and crystallized from ethyl acetate to give 2.17 g (30.7%) of the title compound.

後処理

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with an aqueous solution of sodium carbonate
  3. dry with materialdried over sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was purified by silica gel column chromatography
  6. washThe fraction eluted with 8% ethyl acetate in chloroform
  7. customwas collected
  8. customcrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-650ced8df29c4ed4af120a116f7fb3c1
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05008266

反応ノート

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