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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 13772986, 화합물 → HCID 13772988, 화합물

HRID 746007
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HRID 746007 반응식
[CH2:1]([N:3]1[C:11]2[CH:10]=[C:9]3[CH:12]=[CH:13][C:14]([O:18][CH3:19])=[C:15]([O:16][CH3:17])[C:8]3=[C:7]3[CH:20]=[C:21]([CH3:23])[CH:22]=[C:5]([C:6]=23)[C:4]1(O)[CH2:24][CH2:25][CH3:26])[CH3:2]>C(O)C.[Zn].[Hg](Cl)Cl>[CH2:1]([N:3]1[C@@H:11]2[C:6]3=[C:7]([CH:20]=[C:21]([CH3:23])[CH:22]=[C:5]3[C@H:4]1[CH2:24][CH2:25][CH3:26])[C:8]1[C:15]([O:16][CH3:17])=[C:14]([O:18][CH3:19])[CH:13]=[CH:12][C:9]=1[CH2:10]2)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 13772986HCID 13772986, 화합물

생성물 1

HCID 13772988HCID 13772988, 화합물

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 24085Mercuric Chloride촉매HCID 702Ethanol용매

실험 절차

A suspension of 100 g (0.273M) of 5-ethyl-4,5-dihydro-4-hydroxy-9,10-dimethoxy-2-methyl-4-n-propyl-dibenz[cd,f]indole in 2000 ml ethanol is added with stirring to a suspension of 322 g (4.928M) of zinc dust and 74.3 g (0.273M) of mercury(II) chloride in 2000 ml distilled water. The reaction mixture is refluxed, 450 ml of 18% hydrochloric acid are added dropwise over a period of 15 minutes and the mixture is refluxed overnight with stirring. The mixture is then cooled to room temperature, filtered and the zinc amalgam is washed with 500 ml methylene chloride. The filtrate is made alkaline with 1 liter of concentrated NH4OH and extracted three times with methylene chloride (700 ml each time). The combined organic phases are washed with water, dried and evaporated. The resultant oil is chromatographed on silica gel using methylene chloride with 2% methanol to give the title compound as an oil.

후처리

  1. additionis added
  2. distillationdistilled water
  3. temperatureThe reaction mixture is refluxed
  4. addition450 ml of 18% hydrochloric acid are added dropwise over a period of 15 minutes
  5. temperaturethe mixture is refluxed overnight
  6. filtrationfiltered
  7. washthe zinc amalgam is washed with 500 ml methylene chloride
  8. extractionextracted three times with methylene chloride (700 ml each time)
  9. washThe combined organic phases are washed with water
  10. customdried
  11. customevaporated
  12. customThe resultant oil is chromatographed on silica gel

출처 및 근거

ORD 기록
ord-bffd74ca52984c9f81f0846317d04f99
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04602032

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