Triethylamine → 3,6-dichloro-N-[4-(dimethylphosphoryl)phenyl]-1,2,4-triazin-5-amine

HRID 1472107ノート

反応式

HRID 1472107 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([P:8](=[O:11])([CH3:10])[CH3:9])=[CH:4][CH:3]=1.[Cl:12][C:13]1[N:14]=[N:15][C:16]([Cl:20])=[C:17](Cl)[N:18]=1.C(N(CC)CC)C>C(Cl)Cl>[Cl:12][C:13]1[N:14]=[N:15][C:16]([Cl:20])=[C:17]([NH:1][C:2]2[CH:3]=[CH:4][C:5]([P:8]([CH3:9])([CH3:10])=[O:11])=[CH:6][CH:7]=2)[N:18]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 122624033,5,6-Trichloro-1,2,4-triazineHCID 206345534-(Dimethylphosphoryl)aniline

生成物 1

HCID 866688243,6-dichloro-N-[4-(dimethylphosphoryl)phenyl]-1,2,4-triazin-5-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 4-amino-dimethylphenylphosphine oxide (1.6 mmol) and 3,5,6-trichloro-1,2,4-triazine (1.6 mmol) in CH2Cl2, is added triethylamine (2 mmol). The reaction mixture is allowed to cool to room temperature, dissolved in dichloromethane and washed with an aqueous solution of Na2CO3. The dichloromethane extract is dried over MgSO4 and evaporated. The crude product is purified by Prep-HPLC.

後処理

  1. washwashed with an aqueous solution of Na2CO3
  2. extractionThe dichloromethane extract
  3. dry with materialis dried over MgSO4
  4. customevaporated
  5. customThe crude product is purified by Prep-HPLC

出典と根拠

ORDレコード
ord-b5173b9c7aa644cda798faf1be963748
出典データセット
uspto-grants-2015_04
特許番号
US09012462B2

反応ノート

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