三乙胺 → 5-乙氧基-2-吲哚酮

HRID 2197

反应方程式

HRID 2197 反应方程式
C[CH2:2][C:3]([O:5]CC)=S.ClCl.[CH2:10]([O:12][C:13]1[CH:19]=[CH:18][C:16]([NH2:17])=[CH:15][CH:14]=1)[CH3:11].C(N(CC)CC)C>C(Cl)Cl.O>[CH2:10]([O:12][C:13]1[CH:19]=[C:18]2[C:16](=[CH:15][CH:14]=1)[NH:17][C:3](=[O:5])[CH2:2]2)[CH3:11]

参与物

7

反应物 4

HCID 8471三乙胺HCID 9076对乙氧基苯胺HCID 245262,6-二氯-4-硝基苯胺HCID 12284386Ethyl methylthioacetate

产物 1

HCID 113558125-乙氧基-2-吲哚酮

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6344二氯甲烷溶剂3 次

实验过程

23.6 g of ethyl methylthioacetate in 60 ml of DCM are added to a solution, cooled to about -70° C., of 12.5 g of chlorine in 400 ml of DCM. After stirring for 5 minutes at the same temperature, a solution of 4-ethoxyaniline (48.3 g) in 120 ml of DCM is added. The mixture is stirred for one hour at about -70° C., 39.3 ml of triethylamine are added and the resulting mixture is allowed to warm up to room temperature. 200 ml of water are added and the organic phase is decanted, dried over magnesium sulfate and evaporated under reduced pressure. The residue is taken up with 500 ml of isopropanol and 20 ml of concentrated hydrochloric acid. The mixture is stirred for about 16 hours at room temperature and filtered and the precipitate is separated off. The filtrate is concentrated under reduced pressure to give the expected product.

后处理

  1. stirringThe mixture is stirred for one hour at about -70° C.
  2. customthe organic phase is decanted
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure
  5. stirringThe mixture is stirred for about 16 hours at room temperature
  6. filtrationfiltered
  7. customthe precipitate is separated off
  8. concentrationThe filtrate is concentrated under reduced pressure

来源与证据

ORD记录
ord-137bd4435e364643b101a1a71a0e2096
来源数据集
uspto-grants-1998_03
专利号
US05728723

关联笔记

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