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

Imidazole → HCID 18467051, 화합물

HRID 2229251
노트
인쇄 미리보기

반응식

HRID 2229251 반응식
O[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:16]=[CH:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=1)=[O:6].C(N(CC)CC)C.CS(Cl)(=O)=O.[NH:29]1[CH:33]=[CH:32][N:31]=[CH:30]1>C1COCC1.[Na+].[I-].O>[N:29]1([CH2:2][CH2:3][CH2:4][C:5]([C:7]2[CH:16]=[CH:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH:8]=2)=[O:6])[CH:33]=[CH:32][N:31]=[CH:30]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 795ImidazoleHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 184670444-Hydroxy-1-(2-naphthyl)-1-butanone

생성물 1

HCID 18467051HCID 18467051, 화합물수율 22.7%

시약·촉매·용매 3

HCID 5238Sodium Iodide촉매
HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a cooled (0° C.) solution of 4-hydroxy-1-(2-naphthyl)-1-butanone (4.32 g) in THF (60 ml) were added triethylamine (5.6 ml) and methanesulfonyl chloride (2.4 ml) successively. The mixture was stirred at 0° for 1 hour. Imidazole (2.93 g) and NaI (0.02 g) were added to the mixture and resulting mixture was refluxed for 16 hours. Water was added and the mixture was concentrated. The residue was extracted with ethyl acetate and the extract was washed with water and brine, dried and concentrated. The residue was chromatographed on silica gel, eluting with ethyl acetate-methanol=20:1, followed by crystallization from ethyl acetate-CH2Cl2-cyclohexane to give the titled compound (1.21 g) as a colorless solid.

후처리

  1. customresulting mixture
  2. temperaturewas refluxed for 16 hours
  3. concentrationthe mixture was concentrated
  4. extractionThe residue was extracted with ethyl acetate
  5. washthe extract was washed with water and brine
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was chromatographed on silica gel
  9. washeluting with ethyl acetate-methanol=20:1
  10. customfollowed by crystallization from ethyl acetate-CH2Cl2-cyclohexane

출처 및 근거

ORD 기록
ord-8de3ba9fd7164ab49ee731895bf7df1e
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06420375B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트