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Phosphorus oxychloride → HCID 18545346, 화합물

HRID 564866
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HRID 564866 반응식
[F:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15]/[CH:16]=[CH:17]/[C:18]3[CH:19]=[N:20][N:21]([C:24]4[CH:29]=[C:28]([CH3:30])[N:27]=[C:26](O)[N:25]=4)[C:22]=3[CH3:23])[CH2:11][CH2:10]2)[CH:5]=[C:6]([F:8])[CH:7]=1.P(Cl)(Cl)([Cl:34])=O>>[Cl:34][C:26]1[N:25]=[C:24]([N:21]2[C:22]([CH3:23])=[C:18](/[CH:17]=[CH:16]/[CH2:15][N:12]3[CH2:13][CH2:14][N:9]([C:4]4[CH:3]=[C:2]([F:1])[CH:7]=[C:6]([F:8])[CH:5]=4)[CH2:10][CH2:11]3)[CH:19]=[N:20]2)[CH:29]=[C:28]([CH3:30])[N:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178428093HCID 178428093, 화합물

생성물 1

HCID 18545346HCID 18545346, 화합물

반응 조건

온도
60 °C

실험 절차

To 250 mg of the compound obtained in Example 34 was added 5 ml of phosphorus oxychloride. The mixture was stirred at 60° C. for 2.5 hours, followed by concentration. A mixture of the concentrate and water was neutralized with sodium hydrogencarbonate and extracted with chloroform three times. The combined organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was subjected to silica gel column chromatography using chloroform was a developing solution. Concentration of the fraction containing the desired compound gave 180 mg of the title compound.

후처리

  • concentrationfollowed by concentration
  • additionA mixture of the
  • concentrationconcentrate
  • extractionextracted with chloroform three times
  • washThe combined organic layer was washed with a saturated sodium chloride aqueous solution
  • dry with materialdried over anhydrous sodium sulfate
  • customThe solvent was evaporated
  • additionConcentration of the fraction containing the desired compound
  • 출처 및 근거

    ORD 기록
    ord-4cf004a9c039484f82f3612716312647
    출처 데이터셋
    uspto-grants-2001_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06169086A

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