1,2-Dichloroethane → HCID 136337161, 화합물

HRID 1428824노트

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HRID 1428824 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:11](=[N:30][C:31]([O:33]CC)=O)[NH:12][C:13]2[CH:18]=[CH:17][C:16]([O:19][C:20]3[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:23]=[CH:22][CH:21]=3)=[CH:15][CH:14]=2)[CH:10]=1)=[O:5])[CH3:2].ClCCCl>[Ti](Cl)(Cl)(Cl)Cl.CCO>[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:11]2[NH:30][C:31](=[O:33])[C:18]3[C:13](=[CH:14][CH:15]=[C:16]([O:19][C:20]4[C:29]5[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=5)[CH:23]=[CH:22][CH:21]=4)[CH:17]=3)[N:12]=2)[CH:10]=1)=[O:5])[CH3:2]

참가 물질

5

반응물 2

HCID 111,2-DichloroethaneHCID 178473530HCID 178473530, 화합물

생성물 1

HCID 136337161HCID 136337161, 화합물

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 702Ethanol용매

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온도
90 °C

실험 절차

Titanium (IV) chloride (0.86 mL, 7.8 mmol) was added to a solution of 1-{ethoxycarbonylimino-[4-(naphthalen-1-yloxy)-phenylamino]methyl}-1H-pyrazole-4-carboxylic acid ethyl ester (0.74 g, 1.6 mmol) and DCE (10 mL), and the resulting mixture was heated to 90° C. for 16 h. The reaction mixture was cooled to room temperature and poured into 50 mL EtOH. The mixture was stirred for 30 min and the solid precipitate was collected by vacuum filtration (0.46 g, 69%). MS (ESI): mass calcd. for C24H18N4O4, 426.1; m/z found, 427.1 [M+H]+. 1H NMR (400 MHz, DMSO-d6): 12.87 (s, 1H), 8.99 (s, 1H), 8.29 (s, 1H), 8.05 (d, J=7.5 Hz, 1H), 8.02 (d, J=8.3 Hz, 1H), 7.86 (d, J=8.3 Hz, 1H), 7.79 (d, J=7.6 Hz, 1H), 7.70 (dd, J=8.9, 2.9 Hz, 1H), 7.64-7.60 (m, 1H), 7.60-7.53 (m, 2H), 7.39 (d, J=2.8 Hz, 1H), 7.23 (d, J=7.4 Hz, 1H), 4.30 (q, J=7.1 Hz, 2H), 1.32 (t, J=7.1 Hz, 3H).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationthe solid precipitate was collected by vacuum filtration (0.46 g, 69%)

출처 및 근거

ORD 기록
ord-b801f5e286044d34b07c043e15c3e475
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937078B2

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