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Triphosgene → HCID 21890989, 화합물

HRID 721483
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HRID 721483 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][N:7]=[C:6]2[O:15][C:16]1[CH:22]=[CH:21][C:19]([NH2:20])=[C:18]([N+:23]([O-:25])=[O:24])[CH:17]=1.ClC(Cl)(O[C:30](=[O:36])OC(Cl)(Cl)Cl)Cl.[CH3:38][C:39]1[CH:51]=[CH:50][CH:49]=[CH:48][C:40]=1[CH2:41][N:42]1[CH2:46][CH2:45][CH:44]([NH2:47])[CH2:43]1.C(=O)([O-])O.[Na+]>C(N(CC)CC)C.C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][N:7]=[C:6]2[O:15][C:16]1[CH:22]=[CH:21][C:19]([NH:20][C:30]([NH:47][CH:44]2[CH2:45][CH2:46][N:42]([CH2:41][C:40]3[CH:48]=[CH:49][CH:50]=[CH:51][C:39]=3[CH3:38])[CH2:43]2)=[O:36])=[C:18]([N+:23]([O-:25])=[O:24])[CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 94429TriphosgeneHCID 516892Sodium BicarbonateHCID 177554014-[(6,7-Dimethoxy-4-quinazolinyl)oxy]-2-nitroanilineHCID 21890784HCID 21890784, 화합물

생성물 1

HCID 21890989HCID 21890989, 화합물수율 23.3%

시약·촉매·용매 2

HCID 6212
Chloroform
용매
HCID 8471Triethylamine용매

실험 절차

Chloroform (13 ml) and triethylamine (2 ml) were added to 4-[(6,7-dimethoxy-4-quinazolinyl)oxy]-2-nitroaniline (100 mg) to prepare a solution. Triphosgene (96 mg) was added to the solution, and the mixture was stirred at room temperature for 30 min. 1-(2-Methylbenzyl)-3-pyrrolidinamine (83 mg) was then added thereto, and the mixture was stirred at room temperature overnight. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction solution, and the mixture was extracted with chloroform. The extract was washed with saturated brine and was then dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by thin-layer chromatography using chloroform/acetone for development. Diethyl ether was added to the purification product, and the precipitated crystal was collected by filtration and was washed to give the title compound (38 mg, yield 23%).

후처리

  1. customto prepare a solution
  2. stirringthe mixture was stirred at room temperature overnight
  3. extractionthe mixture was extracted with chloroform
  4. washThe extract was washed with saturated brine
  5. dry with materialwas then dried over anhydrous sodium sulfate
  6. customThe solvent was removed by distillation under the reduced pressure
  7. customThe residue was purified by thin-layer chromatography
  8. additionDiethyl ether was added to the purification product
  9. filtrationthe precipitated crystal was collected by filtration
  10. washwas washed

출처 및 근거

ORD 기록
ord-b3e1c613af01458cb226e2f3ef1be1ba
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07135466B2

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