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Ammonium thiocyanate → HCID 22908151、化合物

HRID 1379802
ノート
印刷プレビュー

反応式

HRID 1379802 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 15666Ammonium thiocyanateHCID 801724-Cyanobenzoyl chloride

生成物 1

HCID 22908151HCID 22908151、化合物収率 146.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-f736450e2b1a408daa200f72a8278b7c
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05672712

反応ノート

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