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

HRID 2303358노트

반응식

HRID 2303358 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8082Piperidine용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-1ba66145134c485fa594ac991eb183c1
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06432957B1

반응 노트

불러오는 중…