Potassium thiocyanate → HCID 178527845、化合物

HRID 900731ノート

反応式

HRID 900731 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 178527845HCID 178527845、化合物収率 74.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-ddff7a0be1664111a3fa3873a8a04194
出典データセット
uspto-grants-2008_04
特許番号
US07361669B2

反応ノート

読み込み中…