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2-Methoxyethanol → 4-(4-Chloro-2-fluoroanilino)-7-(2-methoxyethoxy)-6-nitroquinazoline

HRID 1838538
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HRID 1838538 반응식
[Na].[CH3:2][O:3][CH2:4][CH2:5][OH:6].Cl.Cl[C:9]1[CH:18]=[C:17]2[C:12]([C:13]([NH:19][C:20]3[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:21]=3[F:27])=[N:14][CH:15]=[N:16]2)=[CH:11][C:10]=1[N+:28]([O-:30])=[O:29]>C(O)(=O)C.O>[Cl:26][C:23]1[CH:24]=[CH:25][C:20]([NH:19][C:13]2[C:12]3[C:17](=[CH:18][C:9]([O:6][CH2:5][CH2:4][O:3][CH3:2])=[C:10]([N+:28]([O-:30])=[O:29])[CH:11]=3)[N:16]=[CH:15][N:14]=2)=[C:21]([F:27])[CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 80192-MethoxyethanolHCID 5360545SodiumHCID 224782507-Chloro-4-(4-chloro-2-fluoroanilino)-6-nitroquinazoline hydrochloride

생성물 1

HCID 187534234-(4-Chloro-2-fluoroanilino)-7-(2-methoxyethoxy)-6-nitroquinazoline수율 60%

시약·촉매·용매 2

HCID 176Acetic Acid용매
HCID 962
Water
용매

실험 절차

Sodium (148 mg, 6.4 mmol) was added to 2-methoxyethanol (10 ml), the mixture stirred for 15 minutes to give a complete solution and the volatiles removed by evaporation. The residue was dissolved in DMSO (5 ml) and 7-chloro-4-(4-chloro-2-fluoroanilino)-6-nitroquinazoline hydrochloride (500 mg, 1.3 mmol) was added. The mixture was stirred at ambient temperature for 18 hours then diluted with a solution of acetic acid (1 ml) in water (20 ml). The resulting precipitate was collected by filtration, washed with water, dried and purified by column chromatography eluting with methylene chloride/methanol (96/4). The purified product was recrystallised from methylene chloride/isohexane to give 4-(4-chloro-2-fluoroanilino)-7-(2-methoxyethoxy)-6-nitroquinazoline (304 mg, 60%) as a yellow solid.

후처리

  1. customto give a complete solution
  2. customthe volatiles removed by evaporation
  3. dissolutionThe residue was dissolved in DMSO (5 ml)
  4. stirringThe mixture was stirred at ambient temperature for 18 hours
  5. filtrationThe resulting precipitate was collected by filtration
  6. washwashed with water
  7. customdried
  8. custompurified by column chromatography
  9. washeluting with methylene chloride/methanol (96/4)
  10. customThe purified product was recrystallised from methylene chloride/isohexane

출처 및 근거

ORD 기록
ord-a0f60cb3763b4b51bad4b44387df5c47
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06673803B2

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