Potassium thiocyanate → 2-Chloro-5-nitropyrimidin-4-yl thiocyanate

HRID 605858노트

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HRID 605858 반응식
[S-:1][C:2]#[N:3].[K+].[Cl:5][C:6]1[N:11]=[C:10](Cl)[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][N:7]=1>CCO>[Cl:5][C:6]1[N:11]=[C:10]([S:1][C:2]#[N:3])[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][N:7]=1

참가 물질

4

반응물 2

HCID 516872Potassium thiocyanateHCID 5212662,4-Dichloro-5-nitropyrimidine

생성물 1

HCID 210775882-Chloro-5-nitropyrimidin-4-yl thiocyanate수율 78.6%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
0 °C

실험 절차

(compound known, e.g. WO 2003/032994) Potassium thiocyanate (0.97 g, 10 mM) was added to a solution of 2,4-dichloro-5-nitropyrimidine (1.94 g 10, mM) in EtOH (40 mL) cooled to 0° C. via an ice bath. The solution was stirred at 0° C. for 30 min, then the bath was removed and the resulting suspension allowed to come to RT over 60 min, when water (100 mL) was added. The precipitate was collected via filtration, washed with ice cold water, dissolved with DCM, dried (MgSO4), filtered and evaporated to yield the titled compound (1.7 g).

후처리

  1. customthe bath was removed
  2. waitto come to RT over 60 min
  3. additionwhen water (100 mL) was added
  4. filtrationThe precipitate was collected via filtration
  5. washwashed with ice cold water
  6. dissolutiondissolved with DCM
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. customevaporated

출처 및 근거

ORD 기록
ord-37bc1171e9e54777a6a896454bbcf563
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915268B2

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