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HCID 22136184, 화합물 → HCID 22136173, 화합물

HRID 1826827
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인쇄 미리보기

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HRID 1826827 반응식
[CH3:1][O:2][C:3]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH2:15][NH:16][C:17](=O)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[N:7][CH:6]=1)=[O:4]>O=P(Cl)(Cl)Cl>[C:18]1([C:17]2[N:7]3[CH:6]=[C:5]([C:3]([O:2][CH3:1])=[O:4])[C:14]4[C:9]([C:8]3=[CH:15][N:16]=2)=[CH:10][CH:11]=[CH:12][CH:13]=4)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 22136184HCID 22136184, 화합물

생성물 1

HCID 22136173HCID 22136173, 화합물수율 37.7%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

반응 조건

온도
105 °C

실험 절차

A mixture of the product from part 7 (1.97 g) in 10 ml of POCl3 is stirred at 105° C. for two hours, then cooled and concentrated under vacuum. The residue is treated with EtOAc and washed with saturated aqueous NaHCO3 solution and water. The organic solution is dried over Na2SO4, filtered and then concentrated to afford a solid. Recrystallization from 2-propanol yields the title compound as a yellow solid (0.7 g).

후처리

  • temperaturecooled
  • concentrationconcentrated under vacuum
  • additionThe residue is treated with EtOAc
  • washwashed with saturated aqueous NaHCO3 solution and water
  • dry with materialThe organic solution is dried over Na2SO4
  • filtrationfiltered
  • concentrationconcentrated
  • customto afford a solid
  • customRecrystallization from 2-propanol
  • 출처 및 근거

    ORD 기록
    ord-e9e7c06717dd433ab45e8975bc495050
    출처 데이터셋
    uspto-grants-2006_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07053093B2

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