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Triethylamine → HCID 22637127, 화합물

HRID 1348822
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HRID 1348822 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[O:9][C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=2)[N:13]=[CH:12][N:11]=1)[NH2:5].C(N(CC)CC)C.Cl[C:32](Cl)([O:34]C(=O)OC(Cl)(Cl)Cl)Cl.[NH2:43][C:44]1[CH:48]=[C:47]([CH3:49])[O:46][N:45]=1>C(Cl)(Cl)Cl.O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:5][C:32]([NH:43][C:44]2[CH:48]=[C:47]([CH3:49])[O:46][N:45]=2)=[O:34])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=2)[N:13]=[CH:12][N:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 661723-Amino-5-methylisoxazoleHCID 94429TriphosgeneHCID 218905643-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]aniline

생성물 1

HCID 22637127HCID 22637127, 화합물수율 30.2%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6212Chloroform용매2회

실험 절차

3-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]aniline (42 mg) was dissolved in chloroform (2.0 ml) and triethylamine (0.13 ml) to prepare a solution. A solution of triphosgene (19 mg) in chloroform was then added to the solution, and the mixture was stirred at room temperature for 5 min. Next, 3-amino-5-methylisoxazole (14 mg) was added thereto, and the mixture was further stirred at room temperature overnight. Water was added to the reaction solution, and the mixture was subjected to separatory extraction with chloroform. The organic layer was concentrated and was evaporated to dryness. Diethyl ether was added to the resultant solid, and the solution was filtered. The filtrate was concentrated, and methyl alcohol was added to the residue. The resultant crystal was collected by filtration to give the title compound (8.8 mg, yield 15%).

후처리

  1. stirringthe mixture was further stirred at room temperature overnight
  2. extractionthe mixture was subjected to separatory extraction with chloroform
  3. concentrationThe organic layer was concentrated
  4. customwas evaporated to dryness
  5. additionDiethyl ether was added to the resultant solid
  6. filtrationthe solution was filtered
  7. concentrationThe filtrate was concentrated
  8. additionmethyl alcohol was added to the residue
  9. filtrationThe resultant crystal was collected by filtration

출처 및 근거

ORD 기록
ord-06941bd67c7a47d1b3c6f17c4298bacf
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07211587B2

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