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Hydrazine → 4-(4-Chlorophenyl)-6-hydrazinylpyrimidine

HRID 271406
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HRID 271406 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[N:5]=[CH:4][N:3]=1.[NH2:15][NH2:16]>C1COCC1>[Cl:14][C:11]1[CH:12]=[CH:13][C:8]([C:6]2[CH:7]=[C:2]([NH:15][NH2:16])[N:3]=[CH:4][N:5]=2)=[CH:9][CH:10]=1
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 249020894-Chloro-6-(4-chlorophenyl)pyrimidine

생성물 1

HCID 587728354-(4-Chlorophenyl)-6-hydrazinylpyrimidine수율 67.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To a stirred solution of 4-chloro-6-(4-chlorophenyl)pyrimidine (1.25 g, 5.6 mmol) in THF (10 mL) at room temperature under argon was added H2NNH2 (538 mg, 16.8 mmol). The reaction mixture was heated at 60° C. under argon for 2 h. Analysis by HPLC/MS indicated that the reaction was complete. About three fourths of the solvent was evaporated and Et2O (5 mL) was added to the resulting suspension. After stirring at room temperature for 20 min, solid was collected by filtration and further washed with Et2O (15 mL), then dried under vacuum to obtain 831 mg of the title compound as a white solid. HPLC/MS: retention time=1.88 min, [M+H]30 =221.

후처리

  1. customAbout three fourths of the solvent was evaporated
  2. additionEt2O (5 mL) was added to the resulting suspension
  3. filtrationsolid was collected by filtration
  4. washfurther washed with Et2O (15 mL)
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-af32e46d1ffd43f9b6bde54a73e0ae39
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07452892B2

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