Hydrazine → HCID 178478044、化合物

HRID 271094ノート

反応式

HRID 271094 の反応式
Cl[C:2]1[C:7]([C:8]([C:10]2[S:11][CH:12]=[CH:13][CH:14]=2)=O)=[CH:6][N:5]=[C:4]([O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[Cl:22])[N:3]=1.[NH2:23][NH2:24]>C(O)C.C1COCC1>[Cl:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[O:15][C:4]1[N:3]=[C:2]2[NH:23][N:24]=[C:8]([C:10]3[S:11][CH:12]=[CH:13][CH:14]=3)[C:7]2=[CH:6][N:5]=1

参加物

5

反応物 2

HCID 9321HydrazineHCID 59834304[4-Chloro-2-(2-chloro-phenoxy)-pyrimidin-5-yl]-thiophen-2-yl-methanone

生成物 1

HCID 178478044HCID 178478044、化合物収率 47.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

[4-Chloro-2-(2-chloro-phenoxy)-pyrimidin-5-yl]-thiophen-2-yl-methanone (82 mg, 0.23 mmol) was dissolved in a mixture of 10 mL ethanol and 0.5 mL THF, and 15 mg of anhydrous hydrazine was added. The reaction mixture was stirred at room temperature for 10 minutes and then was heated to 80° C. for 20 minutes. Solvent was removed under reduced pressure, and the residue was purified by preparative scale TLC using 1.8% MeOH in methylene chloride to yield 36 mg of 6-(2-Chloro-phenoxy)-3-thiophen-2-yl-1H-pyrazolo[3,4-d]pyrimidine. Mass Spec. M+H=329. Mp=221.3-223.1° C.

後処理

  1. additionwas added
  2. temperaturewas heated to 80° C. for 20 minutes
  3. customSolvent was removed under reduced pressure
  4. customthe residue was purified by preparative scale TLC

出典と根拠

ORDレコード
ord-f5bc9f6426ad4e649940daff72d58820
出典データセット
uspto-grants-2008_11
特許番号
US07452880B2

反応ノート

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