1,2-Dichloroethane → HCID 178454340, 화합물

HRID 1875073노트

반응식

HRID 1875073 반응식
C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[NH2:15][CH2:16][C:17]1[C:18]([F:34])=[C:19]([O:24][C:25]2[CH:26]=[C:27]([CH:30]=[C:31]([Cl:33])[CH:32]=2)[C:28]#[N:29])[C:20]([Cl:23])=[CH:21][CH:22]=1.[CH3:35][C:36]([O:39][C:40]([N:42]([C:52]([O:54][C:55]([CH3:58])([CH3:57])[CH3:56])=[O:53])[C:43]1[NH:44][C:45]([C:49](O)=[O:50])=[C:46]([Br:48])[N:47]=1)=[O:41])([CH3:38])[CH3:37].C(=O)(O)[O-].[Na+]>CN(C=O)C>[CH3:58][C:55]([O:54][C:52]([N:42]([C:43]1[NH:44][C:45]([C:49]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[C:19]([O:24][C:25]3[CH:26]=[C:27]([C:28]#[N:29])[CH:30]=[C:31]([Cl:33])[CH:32]=3)[C:18]=2[F:34])=[O:50])=[C:46]([Br:48])[N:47]=1)[C:40]([O:39][C:36]([CH3:35])([CH3:37])[CH3:38])=[O:41])=[O:53])([CH3:56])[CH3:57]

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 594513923-{[3-(Aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrileHCID 178454342HCID 178454342, 화합물

생성물 1

HCID 178454340HCID 178454340, 화합물수율 40.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

EDC (0.022 g, 0.116 mmol) and HOBT (0.016 g, 0.116 mmol) were added to a solution of 3-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile (0.033 g, 0.106 mmol) and 2-(bis{[(1,1-dimethylethyl)oxy]carbonyl}amino)-4-bromo-1H-imidazole-5-carboxylic acid (0.043 g, 0.106 mmol) in DMF (2 mL). The mixture was stirred at RT overnight. Saturated sodium bicarbonate was added and the reaction mixture was extracted with EtOAc. The organic layer was dried over sodium sulfate and concentrated. Chromatography (MeOH:dichloromethane) gave the desired product (0.030 g, 34%) as a white solid.

후처리

  1. extractionthe reaction mixture was extracted with EtOAc
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c1f1415dcaaf412f98139af85d6eb47b
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304419B2

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