Phosphorus oxychloride → HCID 19375606、化合物

HRID 2211101ノート

反応式

HRID 2211101 の反応式
[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9](=O)[NH:8][N:7]=2)=[CH:2]1.P(Cl)(Cl)([Cl:19])=O>ClC(Cl)C>[Cl:19][C:9]1[C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:6]([C:3]2[CH:4]=[CH:5][S:1][CH:2]=2)=[N:7][N:8]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 19375607HCID 19375607、化合物

生成物 1

HCID 19375606HCID 19375606、化合物

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

反応条件

温度
100 °C

実験手順

500 mg of 4-(3-thienyl)-1-phthalazinone and 3 ml of phosphorus oxychloride were dissolved in 6 ml of dichloroethane, and the solution was stirred at 100° C. for 4 hours. The reaction solution was distilled off, and a 1-N aqueous NaOH solution was added thereto under cooling with ice. The solution was extracted with chloroform and dried over magnesium sulfide. The solvent was then distilled off, thereby obtaining 515 mg of 1-chloro-4-(3-thienyl)phthalazine.

後処理

  1. distillationThe reaction solution was distilled off
  2. additiona 1-N aqueous NaOH solution was added
  3. temperatureunder cooling with ice
  4. extractionThe solution was extracted with chloroform
  5. dry with materialdried over magnesium sulfide
  6. distillationThe solvent was then distilled off

出典と根拠

ORDレコード
ord-70d91eeaabdc4a6bb4faa7d1f9c5bdd3
出典データセット
uspto-grants-1995_10
特許番号
US05462941

反応ノート

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