Hydrazine hydrate (1:1) → HCID 20805788、化合物

HRID 631862

反応式

HRID 631862 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1.O.[NH2:16][NH2:17]>O1CCOCC1>[Cl:1][C:2]1[N:7]=[C:6]([NH:16][NH2:17])[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 2415542,4-Dichloro-6-phenylpyrimidine

生成物 1

HCID 20805788HCID 20805788、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 2,4-dichloro-6-phenylpyrimidine (224 mg, 1 mmol) in 1 mL of 1,4-dioxane was added 300 uL of hydrazine hydrate. Stirring was continued at room temperature and the reaction monitored by thin layer chromatography (30% ethyl acetate/hexanes). When the starting material was consumed, 2 mL of water was added and the resultant precipitate was collected on a filter to afford 2-chloro-4-hydrazinyl-6-phenylpyrimidine as a yellow solid. The damp solid was suspended in 2 mL of ethanol, to which was added 220 mg of 4-trifluoromethoxybenzaldehyde. Within 5 minutes the solution became clear and then reprecipitated material. The product, 2-chloro-4-phenyl-6-(2-(4-(trifluoromethoxy)benzylidene)hydrazinyl)pyrimidine (XX), was collected by filtration and dried to afford 150 mg of a solid. ESI/MS 392.973, 395.002 (M+H).

後処理

  1. customwas continued at room temperature
  2. customWhen the starting material was consumed
  3. addition2 mL of water was added
  4. customthe resultant precipitate was collected on
  5. filtrationa filter

出典と根拠

ORDレコード
ord-d54cb5e4acd243dd83d68ec7933d6462
出典データセット
uspto-grants-2016_04
特許番号
US09321735B2

関連ノート

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