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

Hydrochloric Acid → 3,5-dimethyl-4-hydroxy-6-(5-(5-pyrimidinylmethoxy)benzofuran-2-yl)-2H-pyran-2-one

HRID 1357213
노트
인쇄 미리보기

반응식

HRID 1357213 반응식
C(P(CCCC)CCCC)CCC.CN(C(/N=N/C(N(C)C)=O)=O)C.C([O:29][C:30]1[C:35]([CH3:36])=[C:34]([C:37]2[O:38][C:39]3[CH:45]=[CH:44][C:43](O)=[CH:42][C:40]=3[CH:41]=2)[O:33][C:32](=[O:47])[C:31]=1[CH3:48])(=O)C.[OH:49][CH2:50][C:51]1[CH:52]=[N:53][CH:54]=[N:55][CH:56]=1.[OH-].[Li+].Cl>C1COCC1.C(Cl)Cl.CCOC(C)=O>[CH3:48][C:31]1[C:32](=[O:47])[O:33][C:34]([C:37]2[O:38][C:39]3[CH:45]=[CH:44][C:43]([O:49][CH2:50][C:51]4[CH:52]=[N:53][CH:54]=[N:55][CH:56]=4)=[CH:42][C:40]=3[CH:41]=2)=[C:35]([CH3:36])[C:30]=1[OH:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 6

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 13831TributylphosphineHCID 5353800DiamideHCID 15466386(Pyrimidin-5-yl)methanolHCID 185058904-acetyloxy-3,5-dimethyl-6-(5-hydroxybenzofuran-2-yl)-2H-pyran-2-one

생성물 1

HCID 54738107
3,5-dimethyl-4-hydroxy-6-(5-(5-pyrimidinylmethoxy)benzofuran-2-yl)-2H-pyran-2-one

시약·촉매·용매 3

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of tributylphosphine in 2 N THF (0.94 ml) and a solution of TMAD (323 mg) in CH2Cl2 (3 ml) were added dropwise to a solution of 4-acetyloxy-3,5-dimethyl-6-(5-hydroxybenzofuran-2-yl)-2H-pyran-2-one (118 mg) and 5-hydroxymethylpyrimidine (202 mg) in THF (30 ml) at 0° C., and the mixture was stirred at room temperature overnight. The reaction solution was cooled on ice, a 1 N lithium hydroxide aqueous solution (5 ml) was added and the mixture was stirred at room temperature for one hour, after which the reaction solution was again cooled on ice, a 1 N hydrochloric acid aqueous solution (5 ml) and AcOEt were added, the organic layer and aqueous layer were separated, and the aqueous layer was further extracted with AcOEt. The organic layers were combined and dried with MgSO4, and then filtered and concentrated. The residue was purified by silica gel column chromatography (AcOEt/MeOH=10/1) to obtain 3,5-dimethyl-4-hydroxy-6-(5-(5-pyrimidinylmethoxy)benzofuran-2-yl)-2H-pyran-2-one.

후처리

  1. temperatureThe reaction solution was cooled on ice
  2. stirringthe mixture was stirred at room temperature for one hour
  3. temperatureafter which the reaction solution was again cooled on ice
  4. customthe organic layer and aqueous layer were separated
  5. extractionthe aqueous layer was further extracted with AcOEt
  6. dry with materialdried with MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel column chromatography (AcOEt/MeOH=10/1)

출처 및 근거

ORD 기록
ord-81a702c01d49401bb595755b1d9d5695
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06589984B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트