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

HRID 1033161ノート

反応式

HRID 1033161 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-111766c06f1c49099b4d4be7a08e703c
出典データセット
uspto-grants-1994_05
特許番号
US05310723

反応ノート

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