Sodium ethoxide → HCID 178505574, 화합물

HRID 2117732노트

반응식

HRID 2117732 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]3[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=3)=[N:10][C:11](=[S:13])[N:12]=2)=[CH:4][CH:3]=1.[O-]CC.[Na+]>CO>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[NH:12][C:11]([SH:13])=[N:10][C:9]=2[C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 2723922Sodium ethoxideHCID 18461195HCID 18461195, 화합물

생성물 1

HCID 178505574HCID 178505574, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Under an atmosphere of argon, 5-(4-fluorophenyl)-4-(4-pyridinyl)imidazole-2-thione (0.001 mol/0.271 g) was dissolved in 20 ml of absolute methanol. Sodium ethoxide (0.0012 mol/0.065 g) was then added and the mixture was stirred for 10 min. The bromoaliphatic compound (0.0011 mol) in question, dissolved in 10 ml of absolute methanol, was added dropwise to the initial charge. The mixture was then heated under reflux for 4 h and subsequently stirred at room temperature for 2 h. After neutralization with HCl 10% to pH 7, the liquid was removed under reduced pressure and the residue was worked up by column chromatography (mobile phase: CH2Cl2/EtOH 9:1; silica gel).

후처리

  1. additionwas added dropwise to the
  2. additioninitial charge
  3. temperatureThe mixture was then heated
  4. temperatureunder reflux for 4 h
  5. stirringsubsequently stirred at room temperature for 2 h
  6. customAfter neutralization with HCl 10% to pH 7, the liquid was removed under reduced pressure

출처 및 근거

ORD 기록
ord-9f04684da3784c6ba56352e6e88d5056
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07442713B2

반응 노트

불러오는 중…