反応式
C(O[C:4]([C:6]1[C:7]([N:18]([CH3:23])[CH2:19][CH2:20][C:21]#[N:22])=[N:8][C:9]2[C:14]([CH:15]=1)=[CH:13][C:12]([F:16])=[C:11]([F:17])[CH:10]=2)=[O:5])C.CC([O-])(C)C.[K+].C(O)(=O)C.C(O)C.O>O1CCCC1>[C:21]([CH:20]1[CH2:19][N:18]([CH3:23])[C:7]2[N:8]=[C:9]3[CH:10]=[C:11]([F:17])[C:12]([F:16])=[CH:13][C:14]3=[CH:15][C:6]=2[C:4]1=[O:5])#[N:22]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- -10 °C
実験手順
A solution of 19.17 g of 3-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(β-cyanoethyl)amino]quinoline in 50 cm3 of tetrahydrofuran is introduced in the course of 60 minutes into a solution, cooled to -10° C., of 8.74 g of potassium tert-butylate in 200 cm 3 of tetrahydrofuran. The suspension obtained is stirred, still at -10° C., for a further 30 minutes. 4 cm3 of glacial acetic acid are then .introduced. The tetrahydrofuran is evaporated off under reduced pressure (20 kPa). The crude reaction mixture is taken up with 200 cm3 of an aqueous-alcoholic ethanol/water (70/30 vol/vol) mixture. The precipitate obtained is filtered off, washed with twice 50 cm3 of water and then dried under reduced pressure (20 kPa). 16.1 g of 3-cyano-7,8-difluoro-1-methyl-4-oxo-1,2,3,4tetrahydrobenzo[b][1,8]naphthyridine are isolated in the form of a golden-yellow solid, melting point 144° C.
後処理
- customThe suspension obtained
- customThe tetrahydrofuran is evaporated off under reduced pressure (20 kPa)
- customThe crude reaction mixture
- customThe precipitate obtained
- filtrationis filtered off
- washwashed with twice 50 cm3 of water
- customdried under reduced pressure (20 kPa)
出典と根拠
- ORDレコード
- ord-1a1ac345f45244798de9be8861e58aad
- 出典データセット
- uspto-grants-1996_01
- 特許番号
- US05484921
関連ノート
読み込み中…