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

Methyl iodide → Methyl 4-iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cycloheptene-1-carboxylate

HRID 132997
노트
인쇄 미리보기

반응식

HRID 132997 반응식
[I:1][C:2]1[C:7]2[C:8](=[O:19])[C:9]3[CH:16]=[CH:15][CH:14]=[C:13](C=O)[C:10]=3[CH2:11][CH2:12][C:6]=2[CH:5]=[CH:4][CH:3]=1.Cl[O-].[Na+].[CH3:23]I.[C:25](=[O:28])([O-])[O-:26].[K+].[K+]>CN(C)C=O.O>[I:1][C:2]1[C:7]2[C:8](=[O:19])[C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[CH2:11][CH2:12][C:6]=2[C:5]([C:25]([O:26][CH3:23])=[O:28])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 23665760Sodium HypochloriteHCID 586468486-Iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cycloheptene-1-carboxaldehyde

생성물 1

HCID 58646843Methyl 4-iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cycloheptene-1-carboxylate

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

120 mg of the mixture of 6-iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cycloheptene-1-carboxaldehyde and its 4-iodo form prepared in Example 6-b was oxidized by the procedure of Example 4 using sodium hypochlorite. The resulting carboxylic acids were dissolved in 10 ml of N,N-dimethylformamide, and 0.03 ml of methyl iodide and 70 mg of potassium carbonate were added, followed by stirring at room temperature for 2 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:hexane=1:10), to give 110 mg of a mixture of the title compounds as a colorless oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated
  5. customThe residue was purified
  6. customseparated by silica gel column chromatography (ethyl acetate:hexane=1:10)

출처 및 근거

ORD 기록
ord-b6aa85c368104e45aa57232087716090
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07390797B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트