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

Imidazole → 1-(1,2,3,4-Tetrahydronaphthalen-2-yl)imidazole

HRID 863070
노트
인쇄 미리보기

반응식

HRID 863070 반응식
CS(O[CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)(=O)=O.[NH:16]1[CH:20]=[CH:19][N:18]=[CH:17]1>CN(C=O)C>[CH2:7]1[C:8]2[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:14][CH2:15][CH:6]1[N:16]1[CH:20]=[CH:19][N:18]=[CH:17]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 795ImidazoleHCID 218878371,2,3,4-Tetrahydronaphthalen-2-yl methanesulfonate

생성물 1

HCID 132878261-(1,2,3,4-Tetrahydronaphthalen-2-yl)imidazole수율 37,500%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1,2,3,4-tetrahydronaphthalen-2-yl methanesulfonate (15.74 g, 69.6 mmol), prepared as in Example 7, and imidazole (23.68 g, 349 mmol) in 100 mL of DMF was heated at 80° to 90° C. under argon for 24 hours. The solvent was removed under vacuum by rotary evaporation. The residue was dissolved in 500 mL of ethyl acetate and the solution was washed with water (5×250 mL). The combined aqueous layer was extracted with 500 mL of ethyl acetate and the extract was then washed with water (5×250 mL). The combined ethyl acetate extract was washed with saturated sodium chloride solution, dried over magnesium sulfate and concentrated by rotary evaporation. Purification of the residue by column chromatography on silica gel (elution: 5% methanol/methylene chloride) gave 1-(1,2,3,4-tetrahydronaphthalen-2-yl)imidazole (5.18 g, 26.1 mol), m.p. 93°-95° C.

후처리

  1. temperaturewas heated at 80° to 90° C. under argon for 24 hours
  2. customThe solvent was removed under vacuum by rotary evaporation
  3. dissolutionThe residue was dissolved in 500 mL of ethyl acetate
  4. washthe solution was washed with water (5×250 mL)
  5. extractionThe combined aqueous layer was extracted with 500 mL of ethyl acetate
  6. washthe extract was then washed with water (5×250 mL)
  7. extractionThe combined ethyl acetate extract
  8. washwas washed with saturated sodium chloride solution
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated by rotary evaporation
  11. customPurification of the residue by column chromatography on silica gel (elution: 5% methanol/methylene chloride)

출처 및 근거

ORD 기록
ord-a8c9662e759145aa9807ae28704b244e
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05719280

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트