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

HRID 2171554노트

반응식

HRID 2171554 반응식
[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

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178517485HCID 178517485, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 66133Benzyl triethylammonium chloride촉매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-23e2d654830b43d289e6196e8dbe3f19
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051323B2

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