过氧化二苯甲酰 → NCS Chloride

HRID 77495

反应方程式

HRID 77495 反应方程式
FC1C=CC=C(C)N=1.[CH2:9]1[C:14](=[O:15])[N:13]([Cl:16])[C:11](=[O:12])[CH2:10]1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C1C=CC=CC=1>[CH2:9]1[C:14](=[O:15])[N:13]([Cl:16])[C:11](=[O:12])[CH2:10]1.[Cl-:16]

参与物

5

反应物 3

HCID 7187过氧化二苯甲酰HCID 31398N-氯代丁二酰亚胺HCID 960902-氟-6-甲基吡啶

产物 1

HCID 86612418NCS Chloride

试剂、催化剂与溶剂 1

HCID 241苯溶剂

实验过程

2-Fluoro-6-methylpyridine (1.11 g, 10 mmol), NCS (2.0 g, 15 mmol), and catalytic benzoyl peroxide were dissolved in benzene and heated to reflux overnight. The reaction was concentrated and diluted with water and EtOAc. The organic layer was washed with saturated aq. NaHCO3, dried, filtered, and concentrated. The residue was purified on silica gel to give the desired product.

后处理

  1. temperatureheated
  2. temperatureto reflux overnight
  3. concentrationThe reaction was concentrated
  4. additiondiluted with water and EtOAc
  5. washThe organic layer was washed with saturated aq. NaHCO3
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified on silica gel

来源与证据

ORD记录
ord-76c2d06d270544abb8267483dadb4bcd
来源数据集
uspto-grants-2014_09
专利号
US08841295B2

关联笔记

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