(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 → Methyl 3,4-difluoro-2-hydroxybenzoate

HRID 577985笔记

反应方程式

HRID 577985 反应方程式
[F:1][C:2]1[C:3]([OH:12])=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:18]O>O>[F:1][C:2]1[C:3]([OH:12])=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([O:7][CH3:18])=[O:6]

参与物

5

反应物 3

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮HCID 1118四氧化硫HCID 27582863,4-二氟水杨酸

产物 1

HCID 46311128Methyl 3,4-difluoro-2-hydroxybenzoate

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

A solution of 3,4-difluoro-2-hydroxybenzoic acid (6.45 g, 37.05 mmol) and sulfuric acid (6 ml, 113 mmol) in MeOH (25 ml) was heated at reflux overnight. The mixture was diluted with water and extracted with ether. The ether was washed with aqueous NaHCO3, water and brine. The combined aqueous layers were twice more extracted with ether, which was washed with NaHCO3, water, and brine. The combined ether extracts were dried (MgSO4) and concentrated to give 6.4 g of product as a white solid.

后处理

  1. temperatureat reflux overnight
  2. extractionextracted with ether
  3. washThe ether was washed with aqueous NaHCO3, water and brine
  4. extractionThe combined aqueous layers were twice more extracted with ether, which
  5. washwas washed with NaHCO3, water, and brine
  6. dry with materialThe combined ether extracts were dried (MgSO4)
  7. concentrationconcentrated

来源与证据

ORD记录
ord-dc05634c906247dc8ab09044c6c4c294
来源数据集
uspto-grants-2015_05
专利号
US09040528B2

反应笔记

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