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乙酐 → HCID 73031688,化合物

HRID 1663299
笔记
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反应方程式

HRID 1663299 反应方程式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[N:8][N:9]2[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[C:15]([C:19]([F:28])([C:24]([F:27])([F:26])[F:25])[C:20]([F:23])([F:22])[F:21])[CH:16]=3)[NH:11][C:10]2=[O:29])[CH:2]=1.[H-].[Na+].[C:32](OC(=O)C)(=[O:34])[CH3:33]>CC(N(C)C)=O>[C:32]([N:11]1[C:12]2[C:17](=[CH:16][C:15]([C:19]([F:28])([C:24]([F:25])([F:26])[F:27])[C:20]([F:22])([F:21])[F:23])=[CH:14][CH:13]=2)[CH2:18][N:9]([N:8]=[CH:7][C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[C:10]1=[O:29])(=[O:34])[CH3:33]
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 7918乙酐HCID 24758氢化钠HCID 730165883,4-dihydro-3-(3-pyridylmethylideneamino)-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone

产物 1

HCID 73031688HCID 73031688,化合物收率 93.7%

试剂、催化剂与溶剂 1

HCID 31374N,N-二甲基乙酰胺溶剂

实验过程

In 10 ml of dimethylacetamide was dissolved 0.84 g (1.8 mmol) of 3-(3-pyridylmethylideneamino)-3,4-dihydro-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone, and to the resulting solution was added 0.09 g (2.3 mmol) of sodium hydride (purity: 62.4%). The reaction was carried out at room temperature for 30 minutes, after which 0.25 g (2.4 mmol) of acetic anhydride was added and the reaction was carried out for 4 hours. After completion of the reaction, the reaction solution was poured into ice water and the desired compound was extracted with ethyl acetate (20 ml×3). The extract solution was washed with water and saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated in vacuo. The crude product thus obtained was purified by silica gel column chromatography (ethyl acetate−methanol=10:1) to obtain 0.78 g of the desired compound.

后处理

  1. waitthe reaction was carried out for 4 hours
  2. customAfter completion of the reaction
  3. extractionthe desired compound was extracted with ethyl acetate (20 ml×3)
  4. washThe extract solution was washed with water and saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe crude product thus obtained
  8. customwas purified by silica gel column chromatography (ethyl acetate−methanol=10:1)

来源与证据

ORD记录
ord-ec75481853414e9c95bd9ae8da094b36
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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本页导航参与物实验过程后处理来源与证据反应笔记