Water → HCID 86616333、化合物

HRID 559549ノート

反応式

HRID 559549 の反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]2=O)=[CH:4][CH:3]=1.C([O-])(O)=O.[Na+].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:21].O>O1CCOCC1.C(Cl)Cl>[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]2=[S:21])=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 18453089HCID 18453089、化合物

生成物 1

HCID 86616333HCID 86616333、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

A mixture of 1-(4-iodophenyl)pyridin-2(1H)-one prepared above (0.760 g, 2.56 mmol), NaHCO3 (2.15 g, 25.6 mmol) and P2S5 (2.27 g, 10.2 mmol) in dioxane (20 mL) was heated at 80° C. overnight. After being cooled to room temperature, water and CH2Cl2 were added. The organic layer was separated, washed with brine, dried over Na2SO4, concentrated in vacuo to give 1-(4-iodophenyl)pyridine-2(1H)-thione as a solid (0.752 g). MS 313.8 (M+H).

後処理

  1. temperatureAfter being cooled to room temperature
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9d477dd6ace64dabadb42b167babec0e
出典データセット
uspto-grants-2011_11
特許番号
US08063077B2

反応ノート

読み込み中…