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Hydrochloric Acid → 4-(4-Chloro-2-fluoroanilino)-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline hydrochloride

HRID 238102
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인쇄 미리보기

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HRID 238102 반응식
Cl.C(O)C.[Cl:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([O:18][CH2:19][CH:20]3[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]3)=[C:13]([O:16][CH3:17])[CH:14]=2)[N:9]=[CH:8][N:7]=1.[Cl:27][C:28]1[CH:34]=[CH:33][C:31]([NH2:32])=[C:30]([F:35])[CH:29]=1>C(O)(C)C.CCOCC>[ClH:5].[Cl:27][C:28]1[CH:34]=[CH:33][C:31]([NH:32][C:6]2[C:15]3[C:10](=[CH:11][C:12]([O:18][CH2:19][CH:20]4[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]4)=[C:13]([O:16][CH3:17])[CH:14]=3)[N:9]=[CH:8][N:7]=2)=[C:30]([F:35])[CH:29]=1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 938984-Chloro-2-fluoroanilineHCID 117822304-Chloro-6-methoxy-7-((1-methylpiperidin-4-yl)methoxy)quinazoline

생성물 1

HCID 231333204-(4-Chloro-2-fluoroanilino)-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline hydrochloride수율 89.9%

시약·촉매·용매 2

HCID 3283
Diethyl Ether
용매
HCID 3776Isopropanol용매

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온도
50 °C

실험 절차

3.5M Hydrogen chloride in ethanol (75 μl, 0.26 mmol) was added to a suspension of 4-chloro-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline (80 mg, 0.25 mmol), (prepared as described for the starting material in Example 2c), in isopropanol (3 ml), the mixture was heated to 50° C. and 4-chloro-2-fluoroaniline (44 mg, 0.3 mmol) was added. The mixture was heated at reflux for 30 minutes. After cooling, the mixture was diluted with ether (3 ml). The precipitate was collected by filtration, washed with ether and dried under vacuum to give 4-(4-chloro-2-fluoroanilino)-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline hydrochloride (105 mg, 82%).

후처리

  1. custom(prepared
  2. temperatureThe mixture was heated
  3. temperatureat reflux for 30 minutes
  4. temperatureAfter cooling
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with ether
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-d370166b5619435f9afce9ad5251a956
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642608B2

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