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Phosphorus oxychloride → 4-Chloro-2,6-dihydro-2-methyl-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1-one

HRID 1835152
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HRID 1835152 반응식
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[CH:9][N:10]([CH2:12][C:13]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[CH:16]=[CH:15][CH:14]=3)[CH:11]=[C:5]2[C:4](=O)[NH:3]1.P(Cl)(Cl)([Cl:26])=O>>[Cl:26][C:4]1[C:5]2[C:6](=[CH:9][N:10]([CH2:12][C:13]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[CH:16]=[CH:15][CH:14]=3)[CH:11]=2)[C:7](=[O:8])[N:2]([CH3:1])[N:3]=1
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참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 235032482,3-Dihydro-2-methyl-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1,4(6H)-dione

생성물 1

HCID 235032554-Chloro-2,6-dihydro-2-methyl-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1-one

실험 절차

A suspension of 2,3-dihydro-2-methyl-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazine-1,4(6H)-dione (0.10 g) in phosphorus oxychloride (1 ml) was heated at reflux for 30 minutes and then allowed to cool. The solvent was evaporated, water (25 ml) was added and the mixture was extracted with ethyl acetate (2×25 ml). The organic extracts were dried, filtered and evaporated to give the sub-title compound (0.095 g).

후처리

  1. temperaturewas heated
  2. temperature
at reflux for 30 minutes
  • temperatureto cool
  • customThe solvent was evaporated
  • additionwater (25 ml) was added
  • extractionthe mixture was extracted with ethyl acetate (2×25 ml)
  • customThe organic extracts were dried
  • filtrationfiltered
  • customevaporated
  • 출처 및 근거

    ORD 기록
    ord-04184055b5ba49aabe789d109fd45c87
    출처 데이터셋
    uspto-grants-2004_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06770646B2

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