Potassium Hydroxide → HCID 178526679, 화합물

HRID 601128

반응식

HRID 601128 반응식
[N+:1]([C:4]1[C:5](Cl)=[N:6][CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].NC(N)=[S:13].[OH-].[K+]>C(O)C>[SH:13][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=[CH:7][N:6]=1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 796132-Chloro-3-nitropyridineHCID 2723790Thiourea

생성물 1

HCID 178526679HCID 178526679, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-mercapto-3-nitropyridine was prepared by treating 3-nitro-2-chloro-pyridine (50 g, 0.0317 mol) with thiourea (24 g, 0.0317 mol) in 200 mL of ethanol at reflux for several hours. After the reaction mixture was allowed to cool, 7.19 mL solution of KOH (42.8 g in 115 mL of water) was added and the resulting mixture was heated at reflux for 3 hours. The crude reaction mixture was cooled to room temperature and then concentrated to 50% of its volume in vacuo. After diluting with 300 mL of water, the product was isolated by vacuum filtration as an orange solid that was used without further purification. MS (DCI/NH3) m/z 157 (M+H)+. 1H NMR (300 MHz, DMSO-d6) δ 5.76 (m, 1H), 7.67 (dd, J=8.46, 4.78 Hz, 1H), 8.63 (dd, J=8.46, 1.47 Hz, 1H), 8.73 (dd, J=4.60, 1.65 Hz, 1H).

후처리

  1. temperatureat reflux for several hours
  2. temperatureto cool
  3. temperaturethe resulting mixture was heated
  4. temperatureat reflux for 3 hours
  5. customThe crude reaction mixture
  6. concentrationconcentrated to 50% of its volume in vacuo
  7. additionAfter diluting with 300 mL of water
  8. customthe product was isolated by vacuum filtration as an orange solid that
  9. customwas used without further purification

출처 및 근거

ORD 기록
ord-75cc0655452c4bdea50cfd6e5a58c3ef
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902203B2

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