Triethylamine → 3-(6-Fluoroquinolin-2-on-7-yl)-1-methyl-6-trifluoromethyluracil

HRID 1033161노트

반응식

HRID 1033161 반응식
Cl[CH:2]1[CH2:11][C:10]2[C:5](=[CH:6][C:7]([N:13]3[C:18](=[O:19])[CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[N:15]([CH3:24])[C:14]3=[O:25])=[C:8]([F:12])[CH:9]=2)[NH:4][C:3]1=[O:26].C(N(CC)CC)C>O1CCCC1.C(Cl)Cl>[F:12][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][C:7]=1[N:13]1[C:18](=[O:19])[CH:17]=[C:16]([C:20]([F:22])([F:23])[F:21])[N:15]([CH3:24])[C:14]1=[O:25])[NH:4][C:3](=[O:26])[CH:2]=[CH:11]2

참가 물질

5

반응물 2

HCID 8471TriethylamineHCID 190253833-(3-Chloro-6-fluoro-3,4-dihydroquinolin-2-on-7-yl)-1-methyl-6-trifluoromethyluracil

생성물 1

HCID 190253853-(6-Fluoroquinolin-2-on-7-yl)-1-methyl-6-trifluoromethyluracil수율 97.4%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

A stirred solution of 5.2 grams (0.013 mole) of 3-(3-chloro-6-fluoro-3,4-dihydroquinolin-2-on-7-yl)-1-methyl-6-trifluoromethyluracil and 6.2 grams (0.061 mole) of triethylamine in 200 mL of tetrahydrofuran was concentrated under reduced pressure to a residue. The residue was dissolved in methylene chloride and washed with water. The organic layer was dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, yielding 4.5 grams of 3-(6-fluoroquinolin-2-on-7-yl)-1-methyl-6-trifluoromethyluracil, mp 179° C., dec. The NMR spectrum was consistent with the proposed structure.

후처리

  1. washwashed with water
  2. dry with materialThe organic layer was dried with magnesium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-111766c06f1c49099b4d4be7a08e703c
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310723

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