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Ethanol → HCID 44215053, 화합물

HRID 1532365
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HRID 1532365 반응식
C(OC(=O)[N:10]([CH2:21][CH2:22][C:23]1[C:31]2[C:26](=[CH:27][CH:28]=[C:29]([C:32]([CH3:43])([CH3:42])[C:33]([N:35]3[CH:39]4[CH2:40][CH2:41][CH:36]3[CH2:37][CH2:38]4)=[O:34])[CH:30]=2)[NH:25][C:24]=1[C:44]1[CH:49]=[C:48]([CH3:50])[CH:47]=[C:46]([CH3:51])[CH:45]=1)[CH2:11][CH2:12][CH2:13][CH2:14][C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)C1C=CC=CC=1.C(O)C.C(OCC)(=O)C.[H][H]>[Pd].C(Cl)Cl.CO>[CH:36]12[N:35]([C:33](=[O:34])[C:32]([C:29]3[CH:30]=[C:31]4[C:26](=[CH:27][CH:28]=3)[NH:25][C:24]([C:44]3[CH:45]=[C:46]([CH3:51])[CH:47]=[C:48]([CH3:50])[CH:49]=3)=[C:23]4[CH2:22][CH2:21][NH:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]3[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=3)([CH3:43])[CH3:42])[CH:39]([CH2:38][CH2:37]1)[CH2:40][CH2:41]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 702EthanolHCID 8857Ethyl AcetateHCID 69951628HCID 69951628, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 44215053HCID 44215053, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매
HCID 21226129
Dichloromethane methanol
용매

실험 절차

A mixture of 80.2 mg (0.115 mmol) of [2-[5-[2-(7-azabicyclo[2.2.1]hept-7-yl)-1,1-dimethyl-2-oxoethyl]-2-(3,5-dimethylphenyl)-1H-indol-3-yl]ethyl]-[4-(pyridin-3yl)butyl]carbamic acid benzyl ester, 40 mg of 10% palladium on carbon, 4 mL of absolute ethanol, and 4 mL of ethyl acetate was shaken with hydrogen (46 psig) in a pressure vessel for 6 hours. The catalyst was removed by filtration through Celite under nitrogen, and the filtrate was concentrated in vacuo at room temperature. The residue was purified by preparative TLC on 4 Analtech tapered silica gel plates (20×20 cm), which were developed in 92.5:7.5:0.75 CH2Cl2-MeOH-concentrated NH4OH. The product band from each plate was isolated, combined, and extracted with 92.5:7.5:0.75 CH2C12-MeOH-concentrated NH4OH. Concentration of the extracts in vacuo yielded 53.8 mg (81%) of a pale yellow, stiff gum or glass; essentially homogeneous by TLC in 92.5:7.5:0.75 CH2Cl2-MeOH-concentrated MeOH-concentrated NH4OH. 500 MHz 1H NMR (CDCl3) was consistent with the assigned structure. Mass spectrum (ESI): m/e=563.5 (M+H).

후처리

  1. customThe catalyst was removed by filtration through Celite under nitrogen
  2. concentrationthe filtrate was concentrated in vacuo at room temperature
  3. customThe residue was purified by preparative TLC on 4 Analtech tapered silica gel plates (20×20 cm), which
  4. customThe product band from each plate was isolated
  5. extractionextracted with 92.5:7.5:0.75 CH2C12-MeOH-concentrated NH4OH
  6. customConcentration of the extracts in vacuo yielded 53.8 mg (81%) of a pale yellow, stiff gum or glass

출처 및 근거

ORD 기록
ord-69241aba780545c1aca03251bbc06db1
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06200957B1

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