Water → 2-methyl-4-nitro-N-(7-chloro-1,8-naphthyridin-2-yl)-benzamide

HRID 328279ノート

反応式

HRID 328279 の反応式
[CH3:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[NH2:14][C:15]1[CH:24]=[CH:23][C:22]2[C:17](=[N:18][C:19]([Cl:25])=[CH:20][CH:21]=2)[N:16]=1.O>N1C=CC=CC=1>[CH3:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([NH:14][C:15]1[CH:24]=[CH:23][C:22]2[C:17](=[N:18][C:19]([Cl:25])=[CH:20][CH:21]=2)[N:16]=1)=[O:5]

参加物

5

反応物 3

HCID 962WaterHCID 851997-Chloro-1,8-naphthyridin-2-amineHCID 128464852-Methyl-4-nitrobenzoyl chloride

生成物 1

HCID 214443672-methyl-4-nitro-N-(7-chloro-1,8-naphthyridin-2-yl)-benzamide収率 94%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

2-Methyl-4-nitro-benzoyl chloride (16.1 g.) is added all at once to a suspension of 2-amino-7-chloro-1,8-naphthyridine (14.5 g.) in pyridine (161 cc.). The temperature rises to 40° C. The mixture is stirred for a further hour and water (640 cc.) is then added. The precipitate is filtered off and washed with water (225 cc.) and then with acetone (150 cc.). After recrystallisation from acetonitrile (1,600 cc.), 2-methyl-4-nitro-N-(7-chloro-1,8-naphthyridin-2-yl)-benzamide (26 g.) melting at 229° C is obtained.

後処理

  1. customrises to 40° C
  2. filtrationThe precipitate is filtered off
  3. washwashed with water (225 cc.)
  4. customAfter recrystallisation from acetonitrile (1,600 cc.)

出典と根拠

ORDレコード
ord-011e71be5ca243c48f335eb02e4e66bc
出典データセット
uspto-grants-1977_04
特許番号
US04016274

反応ノート

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