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Acetic Acid → RP60556A

HRID 1266156
ノート
印刷プレビュー

反応式

HRID 1266156 の反応式
Cl[C:2]1[C:3]([F:21])=[CH:4][C:5]2[C:6]([CH:20]=1)=[N:7][C:8]1[N:9]([CH3:19])[CH:10]=[C:11]([C:16]([OH:18])=[O:17])[C:12](=[O:15])[C:13]=1[CH:14]=2.[F:22][C:23]1[CH:28]=[CH:27][C:26]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)=[CH:25][CH:24]=1.C(O)(=O)C>N1C=CC=CC=1.O>[F:21][C:3]1[C:2]([N:32]2[CH2:31][CH2:30][N:29]([C:26]3[CH:25]=[CH:24][C:23]([F:22])=[CH:28][CH:27]=3)[CH2:34][CH2:33]2)=[CH:20][C:6]2=[N:7][C:8]3[N:9]([CH3:19])[CH:10]=[C:11]([C:16]([OH:18])=[O:17])[C:12](=[O:15])[C:13]=3[CH:14]=[C:5]2[CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 176Acetic AcidHCID 752601-(4-Fluorophenyl)piperazineHCID 147005548-Chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid

生成物 1

HCID 484065RP60556A収率 62.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1049
Pyridine
溶媒

反応条件

温度
115 °C

実験手順

A suspension of 3.07 g of 8-chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid and 7.21 g of 4-(4-fluorophenyl)-piperazine in 30 cm3 of pyridine was heated at a temperature around 115° C. for 84 hours. The reaction mixture was concentrated under reduced pressure (20 kPa) at approximately 60° C. The solid obtained was taken up in 50 cm3 of water and 3.5 cm3 of 10% acetic acid were added. The suspension was brought to approximately 100° C. The solidified product was filtered off and washed 3 times with 30 cm3 and 3 times 30 cm3 of warm ethanol. After recrystallizing twice from 65 cm3 of dimethylformamide on each occasion, 2.82 g of 7-fluoro-8-[4-(4-fluorophenyl)piperazin-1-yl]-1-methyl-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid were obtained in the form of a yellow solid melting at about 318-319° C.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure (20 kPa) at approximately 60° C
  2. customThe solid obtained
  3. customwas brought to approximately 100° C
  4. filtrationThe solidified product was filtered off
  5. washwashed 3 times with 30 cm3 and 3 times 30 cm3 of warm ethanol
  6. customAfter recrystallizing twice from 65 cm3 of dimethylformamide on each occasion

出典と根拠

ORDレコード
ord-f0ae10760f564fe8866a6e911339a3fe
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06548506B2

反応ノート

読み込み中…

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