Potassium thiocyanate → HCID 178527845, 화합물

HRID 900731노트

반응식

HRID 900731 반응식
Cl.[NH2:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)=O.[S-:12][C:13]#[N:14].[K+]>O>[N:9]1[CH:10]=[CH:11][C:6]([C:4]2[N:14]=[C:13]([SH:12])[NH:2][CH:3]=2)=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 516872Potassium thiocyanateHCID 222816172-Amino-1-pyridin-4-yl-ethanone dihydrochloride

생성물 1

HCID 178527845HCID 178527845, 화합물수율 74.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-Amino-1-pyridin-4-yl-ethanone hydrochloride (0.75 g, 4.348 mMol) was dissolved in water (15 mL), and to clear yellow solution was added potassium thiocyanate (0.7 g, 7.203 mMol). The mixture was heated to reflux for 4.0 h during which period HPLC showed complete disappearance of starting material. On cooling to room temperature, a yellow solid precipitate formed, which was collected by filtration. The solid was then re-suspended in a saturated solution of NaHCO3 (30 mL), stirred at room temperature for 0.5 h, and the resulting free base thiol was collected by filtration. The solid was dried under vacuum to yield 576 mg (59%) of a fluorescent yellow solid. MS(ES) 178 (M+H)

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4.0 h during which period HPLC
  3. customa yellow solid precipitate formed
  4. filtrationwhich was collected by filtration
  5. filtrationthe resulting free base thiol was collected by filtration
  6. customThe solid was dried under vacuum

출처 및 근거

ORD 기록
ord-ddff7a0be1664111a3fa3873a8a04194
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07361669B2

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