Water → HCID 178503471, 화합물

HRID 2208990노트

반응식

HRID 2208990 반응식
Cl[C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[CH:5]=[C:4]([Cl:11])[N:3]=1.[CH3:12][S-:13].[Na+].O>CN(C=O)C>[Cl:11][C:4]1[N:3]=[C:2]([S:13][CH3:12])[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[CH:5]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 4378561Sodium methanethiolate3회HCID 178477826HCID 178477826, 화합물

생성물 1

HCID 178503471HCID 178503471, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

To a solution of 4,6-dichloro-3H-imidazo[4,5-c]pyridine (2.01 g, 10.7 mmol) in DMF (21 mL) at room temperature was added sodium methanethiolate (1.88 g, 26.8 mmol). Mixture was heated at 120° C. for eight hours. An additional 801 mg of sodium methanethiolate was added and mixture stirred at 120° C. for fifteen hours. After adding an additional 340 mg of sodium methanethiolate and heating at 120° C. for five hours, reaction mixture was cooled to room temperature and poured into 100 mL of water. This was then extracted with ethyl acetate (5×150 mL) and combined organic layers were washed with 50% Brine (100 mL), dried (Na2SO4), filtered, and concentrated under reduced pressure to yield 6-chloro-4-(methylthio)-3H-imidazo[4,5-c]pyridine 2.01, which was used in the next step without further purification.

후처리

  1. temperatureheating at 120° C. for five hours
  2. customreaction mixture
  3. temperaturewas cooled to room temperature
  4. extractionThis was then extracted with ethyl acetate (5×150 mL)
  5. washwere washed with 50% Brine (100 mL)
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-89cea408a09441dc80d7483f835dd26b
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09376441B2

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