Acetic Acid → HCID 53712035, 화합물

HRID 344861

반응식

HRID 344861 반응식
[F:1][C:2]1[C:21](F)=[CH:20][C:5]2=[N:6][C:7]3[N:8]([O:18][CH3:19])[CH:9]=[C:10]([C:15]([OH:17])=[O:16])[C:11](=[O:14])[C:12]=3[CH:13]=[C:4]2[CH:3]=1.[C:23]1([CH:29]2[CH2:34][NH:33][CH2:32][CH2:31][NH:30]2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.O.C(O)(=O)C>CS(C)=O>[F:1][C:2]1[C:21]([N:33]2[CH2:32][CH2:31][NH:30][CH:29]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH2:34]2)=[CH:20][C:5]2=[N:6][C:7]3[N:8]([O:18][CH3:19])[CH:9]=[C:10]([C:15]([OH:17])=[O:16])[C:11](=[O:14])[C:12]=3[CH:13]=[C:4]2[CH:3]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 2506732-PhenylpiperazineHCID 14853343HCID 14853343, 화합물

생성물 1

HCID 53712035HCID 53712035, 화합물수율 68.3%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
20 °C

실험 절차

A suspension of 7,8-difluoro-1-methoxy-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid (2 g) and (RS)-2-phenylpiperazine (2.1 g) in dimethyl sulphoxide (30 cc) is heated with stirring for 15 minutes to approximately 50° C. After cooling to approximately 20° C., the reaction mixture is poured into water (100 cc) and treated with acetic acid (1.2 cc). The insoluble matter is drained, washed with water (3×10 cc) and recrystallized in dimethylformamide (80 cc). (RS)-7-Fluoro-1-methoxy-4-oxo-8-(3-phenyl-1-piperazinyl)-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid (2 g) is obtained in the form of a yellow solid, decomposing at 284° C.

후처리

  1. temperatureis heated
  2. washwashed with water (3×10 cc)
  3. customrecrystallized in dimethylformamide (80 cc)

출처 및 근거

ORD 기록
ord-cfbe001748004234ba70b60613066247
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05053509

연결된 노트

불러오는 중…