3-Chloroaniline → HCID 22270087、化合物

HRID 488411

反応式

HRID 488411 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].Cl[C:10]1[C:19]2[C:14](=[CH:15][C:16]([F:23])=[C:17]([N+:20]([O-:22])=[O:21])[CH:18]=2)[N:13]=[CH:12][N:11]=1.CCCCCC>O1CCOCC1.C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([NH:5][C:10]2[C:19]3[C:14](=[CH:15][C:16]([F:23])=[C:17]([N+:20]([O-:22])=[O:21])[CH:18]=3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1

参加物

6

反応物 3

HCID 79323-ChloroanilineHCID 8058HexaneHCID 106093584-Chloro-7-fluoro-6-nitroquinazoline

生成物 1

HCID 22270087HCID 22270087、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 2.76 ml of 3-chloroaniline in 7 ml of dioxan is added dropwise to 5.0 g of 4-chloro-7-fluoro-6-nitro-quinazoline in 40 ml of methylene chloride at 15° C. within 15 minutes. The reaction mixture is stirred for a further 15 minutes at this temperature before being poured onto 100 ml of n-hexane for working up. The mixture is stirred for about one hour while cooling with an ice bath, then the precipitate formed is filtered off. The hydrochloride thus obtained is suspended in 30 ml of methanol, made alkaline with triethylamine while cooling with an ice bath and combined with 100 ml of water. The precipitate formed is suction filtered and washed with water. The crude product is purified by chromatography on a silica gel column with methylene chloride/methanol (20:1) as eluant. Yield: 3.50 g (50% of theory), Melting point: 223-225° C. Mass spectrum (ESI*): m/z=319, 321 [M+H]*

後処理

  1. stirringThe mixture is stirred for about one hour
  2. temperaturewhile cooling with an ice bath
  3. customthe precipitate formed
  4. filtrationis filtered off

出典と根拠

ORDレコード
ord-9ad4d352327a47ab8d31988f0e557e3c
出典データセット
uspto-grants-2005_12
特許番号
US06972288B1

関連ノート

読み込み中…