Phosphorus oxychloride → HCID 19375606, 화합물

HRID 2211101노트

반응식

HRID 2211101 반응식
[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

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 19375607HCID 19375607, 화합물

생성물 1

HCID 19375606HCID 19375606, 화합물

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-70d91eeaabdc4a6bb4faa7d1f9c5bdd3
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05462941

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