Hydrochloric Acid → 7-Chloro-6,8-difluoro-3-nitroquinoline

HRID 413041ノート

反応式

HRID 413041 の反応式
[CH2:1]([N+:5]([O-:7])=[O:6])/[CH:2]=[N:3]\O.Cl.N[C:10]1[C:17]([F:18])=[C:16]([Cl:19])[C:15]([F:20])=[CH:14][C:11]=1[CH:12]=O>C(O)C>[Cl:19][C:16]1[C:17]([F:18])=[C:10]2[C:11]([CH:12]=[C:1]([N+:5]([O-:7])=[O:6])[CH:2]=[N:3]2)=[CH:14][C:15]=1[F:20]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 185232552-Amino-4-chloro-3,5-difluorobenzaldehydeHCID 58810166(NZ)-N-(2-nitroethylidene)hydroxylamine

生成物 1

HCID 185233317-Chloro-6,8-difluoro-3-nitroquinoline収率 72.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
35 °C

実験手順

17.4 g of methazonic acid and 60 cm3 of a 37% aqueous hydrochloric acid solution were rapidly added, with stirring, to a solution of 8.7 g of 2-amino-4-chloro-3,5-difluorobenzaldehyde in 300 cm3 of ethanol, while the mixture was maintained at a temperature in the region of 35° C. The mixture was stirred for 16 hours at a temperature in the region of 20° C. The precipitate was dewatered and washed 3 times with 25 cm3 of diethyl ether. 8.1 g of 7-chloro-6,8-difluoro-3-nitroquinoline was obtained in the form of an orange-colored solid, which melted at 174° C.

後処理

  1. washwashed 3 times with 25 cm3 of diethyl ether

出典と根拠

ORDレコード
ord-2de4c20b14274734827d1d000d4e4b44
出典データセット
uspto-grants-2003_05
特許番号
US06566362B2

反応ノート

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