Phosphorus oxychloride → 5-Chloro-7-[2,4-dichlorophenyl][1,2,4]triazolo[1,5-c]pyrimidine

HRID 2171554ノート

反応式

HRID 2171554 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]=[C:13](O)[N:12]2[N:16]=[CH:17][N:18]=[C:11]2[CH:10]=1.P(Cl)(Cl)([Cl:21])=O>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[Cl:21][C:13]1[N:12]2[N:16]=[CH:17][N:18]=[C:11]2[CH:10]=[C:9]([C:3]2[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=2[Cl:1])[N:14]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178517485HCID 178517485、化合物

生成物 1

HCID 593130895-Chloro-7-[2,4-dichlorophenyl][1,2,4]triazolo[1,5-c]pyrimidine

試薬・触媒・溶媒 1

HCID 66133Benzyl triethylammonium chloride触媒

反応条件

温度
120 °C

実験手順

2.07 g (7.4 mmol) of 7-[2,4-dichlorophenyl][1,2,4]triazolo[1,5-c]pyrimidin-5-ol (Example 137A) are introduced into phosphoryl chloride (20 ml), 5.0 g (22 mmol) of benzyltriethylammonium chloride are added, and the reaction mixture is stirred at 120° C. for 16 h. The reaction mixture is concentrated and cautiously poured onto ice, while stirring vigorously, and the mixture is stirred for 10 min. The solid is filtered off with suction. 1100 mg (50% of theory) of the product are obtained.

後処理

  1. additionare added
  2. concentrationThe reaction mixture is concentrated
  3. additioncautiously poured onto ice
  4. stirringwhile stirring vigorously
  5. stirringthe mixture is stirred for 10 min
  6. filtrationThe solid is filtered off with suction
  7. custom1100 mg (50% of theory) of the product are obtained

出典と根拠

ORDレコード
ord-23e2d654830b43d289e6196e8dbe3f19
出典データセット
uspto-grants-2015_06
特許番号
US09051323B2

反応ノート

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