Diethyl (ethoxymethylene)malonate → Diethyl 2-(6-trifluoromethyl-2-pyridylaminomethylene)malonate

HRID 128605

反応式

HRID 128605 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[C:7]([NH2:9])[CH:6]=[CH:5][CH:4]=1.C(O[CH:15]=[C:16]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:17]([O:19][CH2:20][CH3:21])=[O:18])C>>[F:11][C:2]([F:1])([F:10])[C:3]1[N:8]=[C:7]([NH:9][CH:15]=[C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:6]=[CH:5][CH:4]=1

参加物

3

反応物 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 8210242-Amino-6-(trifluoromethyl)pyridine

生成物 1

HCID 19374312Diethyl 2-(6-trifluoromethyl-2-pyridylaminomethylene)malonate

反応条件

温度
95 °C

実験手順

A mixture of 6-trifluoromethylpyridin-2-amine (17.2 g) and diethyl ethoxymethylenemalonate (22.9 g) was heated at 95° C., under vacuum for 8 hours. The mixture was cooled and diluted with petroleum ether b.p. 60°-80° C. (50 ml). The mixture was filtered and the residue was recrystallised from IMS to give diethyl 2-(6-trifluoromethyl-2-pyridylaminomethylene)malonate, m.p. 125°-128° C.

後処理

  1. temperatureThe mixture was cooled
  2. filtrationThe mixture was filtered
  3. customthe residue was recrystallised from IMS

出典と根拠

ORDレコード
ord-2745d60f2e3c4211bec208894ff000c1
出典データセット
uspto-grants-1995_11
特許番号
US05464781

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