聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 6-溴吲哚-3-甲醛

HRID 1399861

反应方程式

HRID 1399861 反应方程式
O=P(Cl)(Cl)Cl.[Br:6][C:7]1[CH:15]=[C:14]2[C:10]([CH:11]=[CH:12][NH:13]2)=[CH:9][CH:8]=1.O.[OH-].[Na+].CN([CH:22]=[O:23])C>>[Br:6][C:7]1[CH:15]=[C:14]2[C:10]([C:11]([CH:22]=[O:23])=[CH:12][NH:13]2)=[CH:9][CH:8]=1

参与物

6

反应物 5

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 6228N,N-二甲基甲酰胺2 次HCID 14798二甲基对苯二胺二盐酸HCID 24813三氯氧磷HCID 6764936-溴吲哚

产物 1

HCID 27948306-溴吲哚-3-甲醛

实验过程

POCl3 (980 mg, 6.4 mmol) was added dropwise to DMF (3 mL) cooled in an ice bath. The mixture was stirred at 0° C. for 30 min before a solution of 6-bromo-1H-indole (1.0 g, 5.1 mmol) in DMF (7 mL) was slowly added at 0° C. The mixture was stirred at room temperature for 3 h before being poured into water and neutralized with 1N NaOH. The crude product was collected by filtration and used in next step without further purification. LCMS (m/z): 224.1 [M+H]+.

后处理

  1. temperaturecooled in an ice bath
  2. additionwas slowly added at 0° C
  3. filtrationThe crude product was collected by filtration
  4. customused in next step without further purification

来源与证据

ORD记录
ord-b11a318bb24540bbb61be046c7947240
来源数据集
uspto-grants-2014_12
专利号
US08906900B2

关联笔记

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