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Phosphorus oxychloride → 4-Chloro-5-phenyl-6-(4-(2-(pyrrolidin-1-yl)ethoxy)phenyl)furo[2,3-d]pyrimidine

HRID 502645
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HRID 502645 반응식
[C:1]1([C:7]2[C:15]3[C:14](=O)[NH:13][CH:12]=[N:11][C:10]=3[O:9][C:8]=2[C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][N:26]3[CH2:30][CH2:29][CH2:28][CH2:27]3)=[CH:19][CH:18]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:33])=O>C1C=CC=CC=1>[Cl:33][C:14]1[C:15]2[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)=[C:8]([C:17]3[CH:18]=[CH:19][C:20]([O:23][CH2:24][CH2:25][N:26]4[CH2:27][CH2:28][CH2:29][CH2:30]4)=[CH:21][CH:22]=3)[O:9][C:10]=2[N:11]=[CH:12][N:13]=1
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참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 586032805-phenyl-6-(4-(2-(pyrrolidin-1-yl)ethoxy)phenyl)furo[2,3-d]pyrimidin-4 (3H)-one

생성물 1

HCID 586032684-Chloro-5-phenyl-6-(4-(2-(pyrrolidin-1-yl)ethoxy)phenyl)furo[2,3-d]pyrimidine

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Into a 50 mL round bottom flask was placed 5-phenyl-6-(4-(2-(pyrrolidin-1-yl)ethoxy)phenyl)furo[2,3-d]pyrimidin-4 (3H)-one 46 (132 mg, 0.329 mmol), and benzene (40 mL). The flask was equipped with a magnetic stir bar, dean-stark trap and a reflux condenser. The reaction was brought to reflux with some of the solvent having been distilled into the dean-stark trap. The reaction was allowed to cool to room temperature and phosphorous oxychloride (300 mg, 1.96 mmol) was added dropwise. The reaction was heated at reflux for 20 hours.

후처리

  1. customInto a 50 mL round bottom flask was placed
  2. customThe flask was equipped with a magnetic stir bar, dean-stark trap and a reflux condenser
  3. temperatureto reflux with some of the solvent
  4. distillationhaving been distilled into the dean-stark trap
  5. temperatureThe reaction was heated
  6. temperatureat reflux for 20 hours

출처 및 근거

ORD 기록
ord-ecd68025f2d54284903088210e28f3a1
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776867B2

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