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Ammonium thiocyanate → HCID 22908151, 화합물

HRID 1379802
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HRID 1379802 반응식
[C:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1)#[N:2].[S-:12][C:13]#[N:14].[NH4+:15]>CC(C)=O>[C:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH:14][C:13]([NH:15][CH2:10][CH2:11][CH2:3][CH2:4][CH2:5][CH3:6])=[S:12])=[O:8])=[CH:5][CH:4]=1)#[N:2]
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참가 물질

4

반응물 2

HCID 15666Ammonium thiocyanateHCID 801724-Cyanobenzoyl chloride

생성물 1

HCID 22908151HCID 22908151, 화합물수율 146.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

4-Cyanobenzoyl chloride (12.5 g) was added to a solution of ammonium thiocyanate (5.8 g) in acetone (125 ml) at room temperature, followed by heating under reflux for 15 minutes. The reaction mixture was ice-cooled, and after removal of the insoluble substance by filtration, the filtrate was evaporated under reduced pressure. To the resulting residue were added toluene (125 ml) and n-hexylamine (11 ml) successively, followed by stirring for 16 hours. The reaction mixture was concentrated under reduced pressure, and the residue was chromatographed on silica gel column (ethyl acetate:methylene chloride=4:96) to give 1-(4-cyanobenzoyl)-3-n-hexylthiourea (16 g).

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 15 minutes
  3. temperaturecooled
  4. customafter removal of the insoluble substance
  5. filtrationby filtration
  6. customthe filtrate was evaporated under reduced pressure
  7. additionTo the resulting residue were added toluene (125 ml) and n-hexylamine (11 ml) successively
  8. concentrationThe reaction mixture was concentrated under reduced pressure
  9. customthe residue was chromatographed on silica gel column (ethyl acetate:methylene chloride=4:96)

출처 및 근거

ORD 기록
ord-f736450e2b1a408daa200f72a8278b7c
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05672712

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