2-Mercaptobenzoic Acid → HCID 85590543, 화합물

HRID 846194노트

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HRID 846194 반응식
[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].[S:11]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]Br)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[S:11]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][S:4][C:3]1[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=1[C:1]([OH:10])=[O:9])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 54432-Mercaptobenzoic AcidHCID 11430Potassium CarbonateHCID 10849841Benzene, [(6-bromohexyl)thio]-

생성물 1

HCID 85590543HCID 85590543, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

Thiosalicylic acid (1.2 g, 0.008 mole) and 6-thio-phenoxyhexylbromide (2.5 g, 0.009 mole) are dissolved in dimethylformamide (50 ml) and the solution is stirred under argon. Potassium carbonate (1.5 g, 0.011 mole) is added carefully to the reaction. After the addition is complete the mixture is slowly warmed to 100° C. The solvents are evaporated, and the residue is dissolved in water, acidified with dilute hydrochloric acid, extracted with ethyl acetate, dried over anhydrous sodium sulfate, filtered, and evaporated. The residue is flash chromatographed on silica gel to give the desired product.

후처리

  1. additionAfter the addition
  2. customThe solvents are evaporated
  3. dissolutionthe residue is dissolved in water
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customchromatographed on silica gel

출처 및 근거

ORD 기록
ord-0eebb9c75f2c40409e1c93330a3b49a7
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05135938

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