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Ethyl Acetoacetate → HCID 59272711, 화합물

HRID 1919569
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HRID 1919569 반응식
Cl.[Cl:2][C:3]1[S:4][CH:5]=[C:6]([C:8]([NH2:10])=[NH:9])[N:7]=1.[Cl:11][C:12]1[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:13]=1[CH:14]=O.[C:21]([O:27][CH2:28][CH3:29])(=[O:26])[CH2:22][C:23]([CH3:25])=O.C([O-])(=O)C.[Na+]>C(O)C>[Cl:2][C:3]1[S:4][CH:5]=[C:6]([C:8]2[NH:10][C:23]([CH3:25])=[C:22]([C:21]([O:27][CH2:28][CH3:29])=[O:26])[CH:14]([C:13]3[CH:16]=[CH:17][C:18]([F:20])=[CH:19][C:12]=3[Cl:11])[N:9]=2)[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8868Ethyl AcetoacetateHCID 1450242-Chloro-4-fluorobenzaldehydeHCID 517045Sodium AcetateHCID 66769369HCID 66769369, 화합물

생성물 1

HCID 59272711HCID 59272711, 화합물수율 33.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2 mmol 2-chloro-4-thiazolformamidine hydrochloride, 2 mmol 2-chloro-4-fluorobenzaldehyde, 2 mmol ethyl acetoacetate and 2.2 mmol sodium acetate were reacted under reflux in 10 ml anhydrous ethanol for 20 hr, concentrated, and then ethyl acetate and water were added to separate the layers. The ethyl acetate layer was dried over anhydrous sodium sulfate, and separated by a column chromatography to obtain 0.28 g of a yellowish crystal with mp 141-143° C.; 1H-NMR (400 MHz, DMSO-d6) δ 1.01-1.05 (3H, m); 2.42 (3H, s); 3.92-3.95 (2H, m); 5.97 (1H, br); 7.16-7.40 (3H, m); 8.09 (1H, s); 9.52 (1H, s); MS (EI) 413.0 (M+).

후처리

  1. concentrationconcentrated
  2. additionethyl acetate and water were added
  3. customto separate the layers
  4. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  5. customseparated by a column chromatography

출처 및 근거

ORD 기록
ord-c8a34c6603f04c8c9f28450051e36866
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08168642B2

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