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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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2,4-Dichlorobenzylamine → N-(2,4-Dichlorobenzyl)-7-[(3RS,5RS)-3,5-dimethylpiperazin-1-yl]-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxamide

HRID 2099315
ノート
印刷プレビュー

反応式

HRID 2099315 の反応式
C(N(CC)C(C)C)(C)C.C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[CH3:43][C@H:44]1[NH:49][C@@H:48]([CH3:50])[CH2:47][N:46]([C:51]2[C:60]([O:61][CH3:62])=[C:59]3[C:54]([C:55](=[O:71])[C:56]([C:68](O)=[O:69])=[CH:57][N:58]3[CH2:63][C:64]([F:67])([F:66])[F:65])=[CH:53][C:52]=2[F:72])[CH2:45]1.[Cl:73][C:74]1[CH:81]=[C:80]([Cl:82])[CH:79]=[CH:78][C:75]=1[CH2:76][NH2:77].C(#N)C>CN(C)C=O.C(OCC)(=O)C>[Cl:73][C:74]1[CH:81]=[C:80]([Cl:82])[CH:79]=[CH:78][C:75]=1[CH2:76][NH:77][C:68]([C:56]1[C:55](=[O:71])[C:54]2[C:59](=[C:60]([O:61][CH3:62])[C:51]([N:46]3[CH2:45][CH:44]([CH3:43])[NH:49][CH:48]([CH3:50])[CH2:47]3)=[C:52]([F:72])[CH:53]=2)[N:58]([CH2:63][C:64]([F:66])([F:67])[F:65])[CH:57]=1)=[O:69]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 14852,4-DichlorobenzylamineHCID 6342AcetonitrileHCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 577941837-(cis-3,5-Dimethylpiperazin-1-yl)-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

生成物 1

HCID 76607220
N-(2,4-Dichlorobenzyl)-7-[(3RS,5RS)-3,5-dimethylpiperazin-1-yl]-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxamide
収率 0.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Under argon, 7.52 g (58.2 mmol) of N,N-diisopropylethylamine and 7.71 g (14.81 mmol) of PyBOP are added to 5.20 g (10.58 mmol) of 7-(cis-3,5-dimethylpiperazin-1-yl)-6-fluoro-8-methoxy-1-(2,2,2-trifluoroethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid hydroformate (Example 31A) and 3.73 g (21.2 mmol) of 2,4-dichlorobenzylamine in 10.7 ml of dimethylformamide and the mixture is stirred at room temperature overnight. The reaction mixture is diluted with 1500 ml of ethyl acetate and washed three times with water. The combined aqueous phases are extracted once with ethyl acetate. The combined organic phases are washed with a saturated sodium chloride solution, dried over sodium sulfate and concentrated. The residue is stirred with 30 ml of acetonitrile. The solid is then collected by filtration and dried under high vacuum. 6.80 mg of the target compound are obtained as a cocrystallisate with 1 eq. of acetonitrile. For smaller quantities the residue after extraction can be purified by preparative HPLC (by one of the methods 5 to 8).

後処理

  1. washwashed three times with water
  2. extractionThe combined aqueous phases are extracted once with ethyl acetate
  3. washThe combined organic phases are washed with a saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. stirringThe residue is stirred with 30 ml of acetonitrile
  7. filtrationThe solid is then collected by filtration
  8. customdried under high vacuum

出典と根拠

ORDレコード
ord-405ae29eece54f16b64592e028ce1f0f
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07569563B2

反応ノート

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