Hydrazine → HCID 178478044, 화합물

HRID 230163노트

반응식

HRID 230163 반응식
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

참가 물질

5

반응물 2

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

생성물 1

HCID 178478044HCID 178478044, 화합물수율 47.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

[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.

후처리

  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

출처 및 근거

ORD 기록
ord-af1a3f2a887e40b09929dec8d56d5730
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566708B2

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