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

Water → (E)-1-[(1R,2R)-1-(3,4-difluorophenyl)-2-hydroxypropyl]-3-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}piperidin-2-one

HRID 1436150
노트
인쇄 미리보기

반응식

HRID 1436150 반응식
[F:1][C:2]1[CH:3]=[C:4]([C@@H:9]([NH:13][C:14](=[O:34])/[C:15](=[CH:20]/[C:21]2[CH:26]=[CH:25][C:24]([N:27]3[CH:31]=[C:30]([CH3:32])[N:29]=[CH:28]3)=[C:23]([F:33])[CH:22]=2)/[CH2:16][CH2:17][CH2:18]Cl)[C@H:10]([OH:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8].[H-].[Na+].O>CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]([C@@H:9]([N:13]2[CH2:18][CH2:17][CH2:16]/[C:15](=[CH:20]\[C:21]3[CH:26]=[CH:25][C:24]([N:27]4[CH:31]=[C:30]([CH3:32])[N:29]=[CH:28]4)=[C:23]([F:33])[CH:22]=3)/[C:14]2=[O:34])[C@H:10]([OH:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24758Sodium hydrideHCID 86612622(E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}valeric acid [(1R,2R)-1-(3,4-difluorophenyl)-2-hydroxypropyl]amide

생성물 1

HCID 57938668(E)-1-[(1R,2R)-1-(3,4-difluorophenyl)-2-hydroxypropyl]-3-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}piperidin-2-one수율 81.8%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

A solution of 4 N hydrogen chloride in ethyl acetate (10 mL) was added to a solution of tert-butyl [(1R,2R)-1-(3,4-difluorophenyl)-2-hydroxypropyl]carbamate (960 mg) in methanol (10 mL) at room temperature, and the reaction solution was stirred at room temperature for 30 minutes. The reaction solution was concentrated under reduced pressure to obtain (1R,2R)-1-amino-1-(3,4-difluorophenyl)propan-2-ol hydrochloride (747 mg). DIEA (1.59 mL), WSC (880 mg), and HOBT (620 mg) were added to a solution of (E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene]valeric acid trifluoroacetate (1.00 g) and (1R,2R)-1-amino-1-(3,4-difluorophenyl)propan-2-ol hydrochloride (612 mg) in DMF (20 mL) at room temperature, and the reaction solution was stirred at room temperature for one hour. Ethyl acetate was added to the reaction solution, which was then sequentially washed with saturated sodium bicarbonate water, water, a saturated ammonium chloride solution, and brine. The resulting organic layer was dried over magnesium sulfate and then concentrated under reduced pressure. The resulting solid was washed with heptane to obtain (E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}valeric acid [(1R,2R)-1-(3,4-difluorophenyl)-2-hydroxypropyl]amide (977 mg). (E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}valeric acid [(1R,2R)-1-(3,4-difluorophenyl)-2-hydroxypropyl]amide (977 mg) was dissolved in DMF (25 mL). 60% sodium hydride (95 mg) was added to the reaction solution at room temperature, and the reaction solution was stirred at room temperature for 30 minutes. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resulting extract was dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: ethyl acetate-methanol system), solidified with ethyl acetate and heptane, and separated by filtration to obtain 740 mg of the title compound. The property values of the compound are as follows.

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. extractionThe resulting extract
  3. dry with materialwas dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: ethyl acetate-methanol system)
  6. customseparated by filtration

출처 및 근거

ORD 기록
ord-0cb0c81653ae4bd68ee9a70a112f66ac
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618960B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트