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

HRID 328279노트

반응식

HRID 328279 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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.)

출처 및 근거

ORD 기록
ord-011e71be5ca243c48f335eb02e4e66bc
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04016274

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