聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 4-[乙基(甲基)氨基]苯甲醛

HRID 1663604笔记

反应方程式

HRID 1663604 反应方程式
F[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[CH3:10][NH:11][CH2:12][CH3:13].C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[CH2:12]([N:11]([C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1)[CH3:10])[CH3:13]

参与物

6

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 11430碳酸钾HCID 12219N-乙基甲基胺HCID 68023对氟苯甲醛

产物 1

HCID 133962824-[乙基(甲基)氨基]苯甲醛收率 89%

试剂、催化剂与溶剂 1

HCID 679二甲基亚砜溶剂

实验过程

To a solution of 4-fluorobenzaldehyde (1.5 g) and methylethylamine (1.56 mL) in dimethylsulfoxide (9 mL) was added potassium carbonate (2.17 g) and the mixture was stirred by using a microwave synthesizer (Biotage LTD.) at 120° C. for 2 hours. Thereto was added water and the mixture was extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated in vacuo. The resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20) to give 4-(N-ethyl-N-methylamino)benzaldehyde (1.89 g, yield: 89%).

后处理

  1. customat 120° C.
  2. customfor 2 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20)

来源与证据

ORD记录
ord-5ed1b6e0df1f4b21b7ae5f6f131b099c
来源数据集
uspto-grants-2011_10
专利号
US08034949B2

反应笔记

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