N,N-二甲基甲酰胺二甲基缩醛 → 4-(3-Dimethylamino-acryloyl)-3-methyl-5-methylsulfanylthiophene-2-carbonitrile

HRID 6849

反应方程式

HRID 6849 反应方程式
[C:1]([C:4]1[C:5]([CH3:13])=[C:6]([C:11]#[N:12])[S:7][C:8]=1[S:9][CH3:10])(=[O:3])[CH3:2].[CH3:14][N:15]([CH:17](OC)OC)[CH3:16]>C(#N)C>[CH3:14][N:15]([CH3:17])[CH:16]=[CH:2][C:1]([C:4]1[C:5]([CH3:13])=[C:6]([C:11]#[N:12])[S:7][C:8]=1[S:9][CH3:10])=[O:3]

参与物

4

反应物 2

HCID 78373N,N-二甲基甲酰胺二甲基缩醛HCID 28201864-Acetyl-3-methyl-5-(methylthio)thiophene-2-carbonitrile

产物 1

HCID 5360484-(3-Dimethylamino-acryloyl)-3-methyl-5-methylsulfanylthiophene-2-carbonitrile

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

To a solution of 4-acetyl-3-methyl-5-methylsulfanyl-thiophene-2-carbonitrile (10 mmol) in acetonitrile (5 mL) was added DMF-DMA (2 mL) and the resulting mixture heated at reflux for 18 hours. The reaction was concentrated and the residue triturated with diethyl ether (20 mL). The suspension was filtered and washed with ether to afford the desired product as a yellow solid.

后处理

  1. temperaturethe resulting mixture heated
  2. temperatureat reflux for 18 hours
  3. concentrationThe reaction was concentrated
  4. customthe residue triturated with diethyl ether (20 mL)
  5. filtrationThe suspension was filtered
  6. washwashed with ether

来源与证据

ORD记录
ord-415fb75af4324233a0dbe7387235e9d9
来源数据集
uspto-grants-2006_08
专利号
US07084159B2

关联笔记

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