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四氧化硫 → 新喹唑啉(间二氮杂苯)类杀虫剂

HRID 1663296
笔记
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反应方程式

HRID 1663296 反应方程式
[C:1]([N:4]1[C:13]2[C:8](=[CH:9][C:10]([C:14]([F:23])([C:19]([F:22])([F:21])[F:20])[C:15]([F:18])([F:17])[F:16])=[CH:11][CH:12]=2)[CH2:7][N:6]([N:24]=[CH:25][C:26]2[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=2)[C:5]1=[O:32])(=[O:3])[CH3:2].S(=O)(=O)(O)O>[C].[Pd].CN(C)C=O>[C:1]([N:4]1[C:13]2[C:8](=[CH:9][C:10]([C:14]([F:23])([C:19]([F:20])([F:21])[F:22])[C:15]([F:17])([F:18])[F:16])=[CH:11][CH:12]=2)[CH2:7][N:6]([NH:24][CH2:25][C:26]2[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=2)[C:5]1=[O:32])(=[O:3])[CH3:2]
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

5

反应物 2

HCID 1118四氧化硫HCID 73031688HCID 73031688,化合物

产物 1

HCID 11842644新喹唑啉(间二氮杂苯)类杀虫剂

试剂、催化剂与溶剂 2

HCID 178418390HCID 178418390,化合物催化剂HCID 6228N,N-二甲基甲酰胺溶剂

反应条件

温度
60 °C

实验过程

In a 200-ml autoclave were placed 9.25 g (20 mmol) of 1-acetyl-3,4-dihydro-3-(3-pyridylmethylideneamino)-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone, 0.21 g (0.05 mmol) of 5% palladium-carbon (containing 50% water), 0.4 g (98%, 4 mmol) of concentrated sulfuric acid and 50 ml of dimethylformamide. They were heated to 60° C. with stirring and the reaction was carried out at a hydrogen pressure of 2 kg/cm2 until the hydrogen absorption rate decreased. After the reaction mixture was cooled to room temperature, the catalyst was removed by filtration. The filtrate was analyzed by high performance liquid chromatography. The result is shown in Table 1 below.

后处理

  1. customthe reaction was carried out at a hydrogen pressure of 2 kg/cm2 until the hydrogen absorption rate
  2. temperatureAfter the reaction mixture was cooled to room temperature
  3. customthe catalyst was removed by filtration

来源与证据

ORD记录
ord-401e2c1d412c4d47ad588a5d44831f78
来源数据集
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08034931B2

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记