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

HRID 271406
ノート
印刷プレビュー

反応式

HRID 271406 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 587728354-(4-Chlorophenyl)-6-hydrazinylpyrimidine収率 67.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af32e46d1ffd43f9b6bde54a73e0ae39
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07452892B2

反応ノート

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