Phosphorus sulfide (P2S5) → 1-Methyl-5-Methoxy-2-Indolinethione

HRID 1086511노트

반응식

HRID 1086511 반응식
C(=O)(O)[O-].[Na+].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[N:13]([CH3:17])[C:12](=O)[CH2:11]2.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:20]>O1CCCC1>[CH3:17][N:13]1[C:14]2[C:10](=[CH:9][C:8]([O:7][CH3:6])=[CH:16][CH:15]=2)[CH2:11][C:12]1=[S:20]

참가 물질

5

반응물 3

HCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 91021941,3-Dihydro-5-methoxy-1-methyl-2H-indol-2-one

생성물 1

HCID 137767581-Methyl-5-Methoxy-2-Indolinethione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

18.5 g (0.22 mol) of sodium bicarbonate are added to a solution of 19.5 g (0.11 mol) of 5-methoxy-1-methyl-2-indolinone prepared according to A. H. BECKETT, R. W. DAISLEY and J. WALKER (Tetrahedron 1968, 24 6093) and 16.5 g (0.037 mol) of phosphorus pentasulfide in 200 ml of tetrahydrofuran. The reaction medium is heated to a temperature of 50° C. for 1 h 30 min and then filtered and concentrated on a water bath under vacuum. The residue is taken up with ice-cold water and the mixture is extracted with methylene chloride. The organic phase is washed with saturated sodium chloride solution, dried and evaporated. The residue is used in the next stage without further treatment.

후처리

  1. customprepared
  2. filtrationfiltered
  3. concentrationconcentrated on a water bath under vacuum
  4. extractionthe mixture is extracted with methylene chloride
  5. washThe organic phase is washed with saturated sodium chloride solution
  6. customdried
  7. customevaporated

출처 및 근거

ORD 기록
ord-5b94579deea04c9a84ebb9428ed474c1
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05030646

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