Sodium Hydroxide → HCID 59007067、化合物

HRID 130404ノート

反応式

HRID 130404 の反応式
[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[N:11]=[C:10]([S:12]([O:15]C3C=CC=CC=3)(=[O:14])=[O:13])[CH:9]=[CH:8][CH:7]=2)=[CH:2]1.[OH-].[Na+:23]>C(O)C>[Na+:23].[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[N:11]=[C:10]([S:12]([O-:15])(=[O:14])=[O:13])[CH:9]=[CH:8][CH:7]=2)=[CH:2]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 59007072HCID 59007072、化合物

生成物 1

HCID 59007067HCID 59007067、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

A mixture of phenyl 6-(3-thienyl)-2-pyridinesulfonate (D8) (634 mg, 2 mmol) and aqueous sodium hydroxide solution (1M, 12 ml) in ethanol (20 ml) was stirred at 60° C. for 18 hours. After cooling to room temperature the solution was concentrated in vacuo. The resulting residue was diluted with water, the pH was adjusted to pH 4-5 with 1M hydrochloric acid and the solution was washed with diethyl ether. The aqueous phase was concentrated in vacuo and the residue purified by reverse phase C18 silica chromatography (water to 1:10 methanol:water) to afford the title product (D9). MS (ES−) m/e 240 [M−Na]−.

後処理

  1. temperatureAfter cooling to room temperature the solution
  2. concentrationwas concentrated in vacuo
  3. additionThe resulting residue was diluted with water
  4. washthe solution was washed with diethyl ether
  5. concentrationThe aqueous phase was concentrated in vacuo
  6. customthe residue purified by reverse phase

出典と根拠

ORDレコード
ord-a616867af2b144f49e8bc7f201330d5a
出典データセット
uspto-grants-2008_06
特許番号
US07381728B2

反応ノート

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