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Hydrazine hydrate (1:1) → 2-Chloro-4,5-bis(4-chlorophenyl)-6-hydrazinylpyrimidine

HRID 271426
ノート
印刷プレビュー

反応式

HRID 271426 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)[N:3]=1.O.[NH2:24][NH2:25]>N1C=CC=CC=1.O>[Cl:1][C:2]1[N:3]=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)[C:5]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[C:6]([NH:24][NH2:25])[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 598347942,4-Dichloro-5,6-bis(4-chlorophenyl)pyrimidine

生成物 1

HCID 587728472-Chloro-4,5-bis(4-chlorophenyl)-6-hydrazinylpyrimidine収率 95.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1049Pyridine溶媒

実験手順

2,4-Dichloro-5,6-bis(4-chlorophenyl)pyrimidine (1.8 g, 4.86 mmol) was dissolved in pyridine (5 mL) and hydrazine monohydrate (0.26 mL, 5.36 mmol) was added. The reaction mixture was stirred at room temperature for 30 min. The reaction mixture was then diluted with water (10 mL) and extracted with EtOAc (10 mL×2). The combined organic extracts were washed with water, followed by saturated aqueous NaCl, dried (MgSO4), and concentrated at reduced pressure to obtain 1.7 g of the title compound, as a mixture with its regioisomer, as a yellow solid. HPLC/MS: title compound retention time=3.261 min, [M+H]30 =365; regioisomer retention time 3.385 min.

後処理

  1. extractionextracted with EtOAc (10 mL×2)
  2. washThe combined organic extracts were washed with water
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated at reduced pressure

出典と根拠

ORDレコード
ord-85d627069afe4dcca3a4f3cda3034ab7
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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