Ethyl Acetate → N-[2-(tert-butyldimethylsilyloxy)ethyl]-N-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]glycine amide

HRID 2303358ノート

反応式

HRID 2303358 の反応式
[Si:1]([O:8][CH2:9][CH2:10][N:11]([CH2:33][C:34]1[CH:39]=[CH:38][N:37]=[C:36]([C:40]2[CH:45]=[C:44]([O:46][CH3:47])[C:43]([O:48][CH3:49])=[C:42]([O:50][CH3:51])[CH:41]=2)[CH:35]=1)[C:12](=[O:32])[CH2:13][NH:14]C(OCC1C2C=CC=CC=2C2C1=CC=CC=2)=O)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C(OCC)(=O)C>C(#N)C.N1CCCCC1>[Si:1]([O:8][CH2:9][CH2:10][N:11]([CH2:33][C:34]1[CH:39]=[CH:38][N:37]=[C:36]([C:40]2[CH:41]=[C:42]([O:50][CH3:51])[C:43]([O:48][CH3:49])=[C:44]([O:46][CH3:47])[CH:45]=2)[CH:35]=1)[C:12](=[O:32])[CH2:13][NH2:14])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 8857Ethyl AcetateHCID 86758398N-[2-(tert-butyldimethylsilyloxy)ethyl]-N-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]-Nalpha-(9-fluorenylmethoxycarbonyl)glycine amide

生成物 1

HCID 86758399N-[2-(tert-butyldimethylsilyloxy)ethyl]-N-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]glycine amide

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8082Piperidine溶媒

実験手順

N-[2-(tert-butyldimethylsilyloxy)ethyl]-N-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]-Nα-(9-fluorenylmethoxycarbonyl)glycine amide (5.15 g) was dissolved in a 20% acetonitrile solution (40 mL) of piperidine, and the solution was stirred at room temperature for 4 hours. Ethyl acetate was added to the reaction mixture, and the mixture was washed with water and saturated brine, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (chloroform:methanol=20:1) to obtain the title compound.

後処理

  1. washthe mixture was washed with water and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel (chloroform:methanol=20:1)

出典と根拠

ORDレコード
ord-1ba66145134c485fa594ac991eb183c1
出典データセット
uspto-grants-2002_08
特許番号
US06432957B1

反応ノート

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