홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Dicyclohexylcarbodiimide → (S)-5-(1-amino-2-methylpropyl)-3-methyl-1,2,4-oxadiazole

HRID 23761
노트
인쇄 미리보기

반응식

HRID 23761 반응식
C([NH:8][C@H:9]([C:13]([OH:15])=O)[CH:10]([CH3:12])[CH3:11])(OC(C)(C)C)=O.C1(N=C=NC2CCCCC2)CCCCC1.[C:31](=[N:34]O)([NH2:33])[CH3:32]>ClCCl.N1C=CC=CC=1>[NH2:8][C@H:9]([C:13]1[O:15][N:34]=[C:31]([CH3:32])[N:33]=1)[CH:10]([CH3:11])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 30926N-HydroxyacetamidineHCID 83693Boc-L-Valine

생성물 1

HCID 29550895(S)-5-(1-amino-2-methylpropyl)-3-methyl-1,2,4-oxadiazole

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매2회

실험 절차

A solution of BOC-L-valine (4.34 g, 20.0 mmol) in dichloromethane (20 mL) was cooled to 0° C. and treated dropwise with a solution of dicyclohexylcarbodiimide (2.06 g, 10.0 mmol) in dichloromethane (5 mL). After 1 hour the white solid which had formed was removed by filtration and the filtrate concentrated under reduced pressure. The residue was dissolved in pyridine (15 mL) and treated with acetamidoxime (488 mg, 6.6 mmol) in pyridine (5 mL) and the mixture heated at reflux for 1 hour. The pyridine was evaporated under reduced pressure and the residue partitioned between ethyl acetate and water. The organic phase was washed several times with water, dried over magnesium sulfate and concentrated. The residue was chromatographed on silica gel using 10% ethyl acetate in hexanes to elute the product (0.62 g, 25%) as a white solid.

후처리

  1. customAfter 1 hour the white solid which had formed
  2. customwas removed by filtration
  3. concentrationthe filtrate concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in pyridine (15 mL)
  5. temperaturethe mixture heated
  6. temperatureat reflux for 1 hour
  7. customThe pyridine was evaporated under reduced pressure
  8. customthe residue partitioned between ethyl acetate and water
  9. washThe organic phase was washed several times with water
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated
  12. customThe residue was chromatographed on silica gel using 10% ethyl acetate in hexanes
  13. washto elute the product (0.62 g, 25%) as a white solid

출처 및 근거

ORD 기록
ord-63c05ebf483642babd18bb6d0f623481
출처 데이터셋
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06852745B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트