Hydrazine → HCID 178478044、化合物

HRID 230163ノート

反応式

HRID 230163 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 TLCusing 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

出典と根拠

ORDレコード
ord-af1a3f2a887e40b09929dec8d56d5730
出典データセット
uspto-grants-2009_07
特許番号
US07566708B2

反応ノート

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