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Acetic Acid → HCID 22632586, 화합물

HRID 2417535
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HRID 2417535 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([N+:17]([O-])=O)=[C:7]([CH:16]=1)[CH2:8][NH:9][CH2:10][C:11]([O:13]CC)=O)#[N:2].[Cl:20][C:21]1[CH:29]=[CH:28][C:24]([C:25](Cl)=[O:26])=[CH:23][CH:22]=1.C(N(CC)CC)C.[H][H].[N:39]1([C:44]([C:46]2[CH:53]=[CH:52][C:49]([CH:50]=O)=[CH:48][CH:47]=2)=[O:45])[CH2:43][CH:42]=[CH:41][CH2:40]1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl.C(OCC)(=O)C.C1COCC1.[Pd]>[Cl:20][C:21]1[CH:29]=[CH:28][C:24]([C:25]([N:9]2[CH2:8][C:7]3[CH:16]=[C:3]([C:1]#[N:2])[CH:4]=[CH:5][C:6]=3[N:17]([CH2:50][C:49]3[CH:48]=[CH:47][C:46]([C:44]([N:39]4[CH2:43][CH:42]=[CH:41][CH2:40]4)=[O:45])=[CH:53][CH:52]=3)[C:11](=[O:13])[CH2:10]2)=[O:26])=[CH:23][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 7

HCID 176Acetic AcidHCID 8471TriethylamineHCID 85014-Chlorobenzoyl chlorideHCID 5049666Sodium triacetoxyborohydrideHCID 226325974-(2,5-dihydro-1H-pyrrol-1-ylcarbonyl)benz-aldehydeHCID 86589888HCID 86589888, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22632586HCID 22632586, 화합물

시약·촉매·용매 4

HCID 23938Palladium촉매HCID 6344Dichloromethane용매4회HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

5.1 g (16.8 mmol) of ethyl (5-cyano-2-nitrobenzyl)aminoacetate was dissolved in 100 ml of dichloromethane. 2.4 ml (19.3 mmol) of 4-chlorobenzoyl chloride and 3.6 ml (25.2 mmol) of triethylamine were added to the obtained solution under cooling with ice, and they were stirred under cooling with ice for 2 hours. After the treatment with dichloromethane as the extracting solvent by an ordinary method, the crude product thus obtained was dissolved in a mixture of 30 ml of ethyl acetate and 30 ml of THF. 300 mg of 10% palladium/carbon was added to the obtained solution and they were stirred in the presence of hydrogen at room temperature for 6 hours. The reaction solution was filtered through Celite. The solvent was evaporated and 1.4 g (3.8 mmol) of the obtained crude product was dissolved in 50 ml of dichloromethane. 834 mg (4.2 mmol) of 4-(2,5-dihydro-1H-pyrrol-1-ylcarbonyl)benzaldehyde and 0.43 ml (7.6 mmol) of acetic acid were added to the obtained solution, and they were stirred at room temperature for 30 minutes. 2.0 g (9.5 mmol) of sodium triacetoxyborohydride was added to the reaction mixture, and they were stirred at room temperature overnight. After the treatment with dichloromethane as the extracting solvent by an ordinary method, the obtained crude product was purified by the silica gel column chromatography to obtain the title compound.

후처리

  1. temperatureunder cooling with ice, and they
  2. temperatureunder cooling with ice for 2 hours
  3. filtrationThe reaction solution was filtered through Celite
  4. customThe solvent was evaporated
  5. custom1.4 g (3.8 mmol) of the obtained crude product
  6. stirringwere stirred at room temperature for 30 minutes
  7. stirringwere stirred at room temperature overnight
  8. customwas purified by the silica gel column chromatography

출처 및 근거

ORD 기록
ord-8d397b82e09f4d78948d1fbc88344c72
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06825191B2

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