Water → HCID 86616333, 화합물

HRID 559549노트

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HRID 559549 반응식
[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

참가 물질

7

반응물 4

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 18453089HCID 18453089, 화합물

생성물 1

HCID 86616333HCID 86616333, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

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온도
80 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9d477dd6ace64dabadb42b167babec0e
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063077B2

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