Potassium Hydroxide → 2-Bromo-6-[(4,6-dimethoxy-2-pyrimidinyl)thio]benzoic acid

HRID 2106967노트

반응식

HRID 2106967 반응식
[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]([SH:11])[C:7]=1[C:8]([OH:10])=[O:9].[OH-].[K+].CS([C:18]1[N:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH3:27])[N:19]=1)(=O)=O>CN(C)C=O>[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]([S:11][C:18]2[N:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH3:27])[N:19]=2)[C:7]=1[C:8]([OH:10])=[O:9]

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 8383634,6-Dimethoxy-2-(methylsulfonyl)pyrimidineHCID 12423631HCID 12423631, 화합물

생성물 1

HCID 150594242-Bromo-6-[(4,6-dimethoxy-2-pyrimidinyl)thio]benzoic acid수율 35%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

7.0 g of 6-bromothiosalicylic acid was dissolved in 20 ml of an aqueous solution of 4.0 g of potassium hydroxide, and then, 6.9 g of 2-methylsulfonyl-4,6-dimethoxypyrimidine and 20 ml of dimethylformamide were added thereto. The mixture was stirred at room temperature for one hour and poured into a large amount of ice water. The aqueous solution was washed with chloroform and then, neutralized with hydrochloric acid. An oily substance thereby released was extracted with diethyl ether. The diethyl ether layer was dried and passed through a FURORIDIL short column. Diethyl ether was distilled off under reduced pressure to obtain 3.9 g of the desired compound as white powder.

후처리

  1. washThe aqueous solution was washed with chloroform
  2. extractionAn oily substance thereby released was extracted with diethyl ether
  3. dry with materialThe diethyl ether layer was dried
  4. distillationDiethyl ether was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-f73cdf7034e646b18316253dd082b57c
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04932999

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