Ethyl 3-(4-cyano-2-nitrophenyl)-2-oxopropanoate → Ethyl 6-cyano-1H-indole-2-carboxylate

HRID 1866233노트

반응식

HRID 1866233 반응식
[CH2:1]([O:3][C:4](=[O:19])[C:5](=O)[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]#[N:14])=[CH:9][C:8]=1[N+:15]([O-])=O)[CH3:2].[H][H]>CCO>[CH2:1]([O:3][C:4]([C:5]1[NH:15][C:8]2[C:7]([CH:6]=1)=[CH:12][CH:11]=[C:10]([C:13]#[N:14])[CH:9]=2)=[O:19])[CH3:2]

참가 물질

4

반응물 2

HCID 10730167Ethyl 3-(4-cyano-2-nitrophenyl)-2-oxopropanoateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 4715002Ethyl 6-cyano-1H-indole-2-carboxylate수율 65.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Add to 1.5 g of 3-(4-cyano-2-nitrophenyl)-2-oxopropionic acid ethyl ester, in EtOH (40 mL) 10% Pd/C (0.45 g) and stir under a hydrogen atmosphere until the theoretical amount of hydrogen is absorbed. Filter the mixture and concentrate the filtrate to afford 1.1 g of crude product. Purify by chromatography on SiO2 and elute with CH2Cl2. Concentrate the desired fractions and vacuum dry the residue over night (40° C.) to afford the title compound (0.8 g) as white crystals, mp 176° C.

후처리

  1. customis absorbed
  2. filtrationFilter the mixture
  3. concentrationconcentrate the filtrate
  4. customto afford 1.1 g of crude product
  5. customPurify by chromatography on SiO2
  6. washelute with CH2Cl2
  7. concentrationConcentrate the desired fractions and vacuum
  8. customdry the residue over night (40° C.)

출처 및 근거

ORD 기록
ord-ae07819a6dc04f73a626bc079a18dc10
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07629376B2

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