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Ethanol → HCID 44215053、化合物

HRID 1532365
ノート
印刷プレビュー

反応式

HRID 1532365 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 8857Ethyl AcetateHCID 69951628HCID 69951628、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 44215053HCID 44215053、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 21226129
Dichloromethane methanol
溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-69241aba780545c1aca03251bbc06db1
出典データセット
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06200957B1

反応ノート

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