2-Propanethiol → 2-(Isopropylthio)benzaldehyde

HRID 1893125노트

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HRID 1893125 반응식
F[C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].C(=O)([O-])[O-].[K+].[K+].[CH3:16][CH:17]([SH:19])[CH3:18]>CN(C=O)C>[CH:17]([S:19][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5])([CH3:18])[CH3:16]

참가 물질

5

반응물 3

HCID 63642-PropanethiolHCID 11430Potassium Carbonate2회HCID 67970o-Fluorobenzaldehyde

생성물 1

HCID 112061372-(Isopropylthio)benzaldehyde수율 89%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

2-fluoro-benzaldehyde (2.00 g, 16.1 mmol), potassium carbonate (2.45 g, 17.1 mmol) and 2-propanethiol (1.35 g, 17.1 mmol) were dissolved in 10.0 mL, DMF in a 50 mL round-bottomed flask under dry nitrogen, topped with a reflux condenser. The reaction mixture was heated to 50° C. for 48 h. After cooling the mixture was added to 50 mL of saturated potassium carbonate solution, and the mixture was extracted with 3×50 mL portions of ether. The extracts were dried with magnesium sulfate and evaporated. The yellow oil residue of the crude product was further purified by chromatography on silica gel using 95:5 petroleum ether (60-80) and dichloromethane as eluent to afford a yellow oil (2.58 g, 89%).

후처리

  1. customtopped with a reflux condenser
  2. temperatureAfter cooling the mixture
  3. extractionthe mixture was extracted with 3×50 mL portions of ether
  4. dry with materialThe extracts were dried with magnesium sulfate
  5. customevaporated
  6. customThe yellow oil residue of the crude product was further purified by chromatography on silica gel using 95:5 petroleum ether (60-80) and dichloromethane as eluent

출처 및 근거

ORD 기록
ord-d2e33ba4a20c43d39c2bd1c4e572ee96
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513151B2

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