Sodium Hydroxide → HCID 59007067, 화합물

HRID 130404노트

반응식

HRID 130404 반응식
[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

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 59007072HCID 59007072, 화합물

생성물 1

HCID 59007067HCID 59007067, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

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]−.

후처리

  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

출처 및 근거

ORD 기록
ord-a616867af2b144f49e8bc7f201330d5a
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07381728B2

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