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Pyridine → HCID 76607225, 화합물

HRID 2099320
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HRID 2099320 반응식
[Cl:1][C:2]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:3]=1[CH2:4][NH:5][C:6]([C:8]1[C:17](=[O:18])[C:16]2[C:11](=[C:12]([O:28][CH3:29])[C:13]([N:20]3[CH2:25][CH:24]([CH3:26])[NH:23][CH:22]([CH3:27])[CH2:21]3)=[C:14]([F:19])[CH:15]=2)[N:10]([CH2:30][C:31]([F:34])([F:33])[F:32])[CH:9]=1)=[O:7].N1C=CC=CC=1.[Cl-].[C:47]([O:52][CH2:53][CH3:54])(=[O:51])[C:48]([O-])=[O:49]>ClCCl.C(OCC)(=O)C>[CH2:53]([O:52][C:47](=[O:51])[C:48]([N:23]1[CH:22]([CH3:27])[CH2:21][N:20]([C:13]2[C:12]([O:28][CH3:29])=[C:11]3[C:16]([C:17](=[O:18])[C:8]([C:6]([NH:5][CH2:4][C:3]4[CH:35]=[CH:36][C:37]([Cl:39])=[CH:38][C:2]=4[Cl:1])=[O:7])=[CH:9][N:10]3[CH2:30][C:31]([F:33])([F:34])[F:32])=[CH:15][C:14]=2[F:19])[CH2:25][CH:24]1[CH3:26])=[O:49])[CH3:54]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1049PyridineHCID 22632797Monoethyl oxalate monochlorideHCID 76607220N-(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

생성물 1

HCID 76607225HCID 76607225, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매
HCID 8857
Ethyl Acetate
용매

실험 절차

200 mg of the compound from Example 37A are dissolved in 3 ml of dichloromethane and 0.26 ml of pyridine and 71 μl of ethyl oxalate chloride are then added. The mixture is stirred at RT for 3 h. For the work-up, the mixture is diluted with ethyl acetate, and extracted by shaking twice with water, once with a saturated sodium hydrogen carbonate solution and once with a saturated sodium chloride solution. The organic phase is dried over sodium sulfate, concentrated in vacuo, and dried under high vacuum. 220 mg of the title compound are obtained.

후처리

  1. extractionextracted
  2. stirringby shaking twice with water, once with a saturated sodium hydrogen carbonate solution and once with a saturated sodium chloride solution
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customdried under high vacuum

출처 및 근거

ORD 기록
ord-77f406cd9c014c2498fa7c3a739e33ee
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07569563B2

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