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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 59389328, 화합물 → HCID 59389308, 화합물

HRID 2357925
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HRID 2357925 반응식
C[Mg]Br.O1CCC[CH2:5]1.[C:9]([C:12]1[CH:30]=[C:15]2[C:16]([C:22]3[CH:23]([CH3:29])[CH2:24][C:25](=[O:28])[NH:26][N:27]=3)=[CH:17][CH:18]=[C:19]([O:20][CH3:21])[N:14]2[N:13]=1)(=[O:11])[CH3:10]>C1COCC1>[OH:11][C:9]([C:12]1[CH:30]=[C:15]2[C:16]([C:22]3[CH:23]([CH3:29])[CH2:24][C:25](=[O:28])[NH:26][N:27]=3)=[CH:17][CH:18]=[C:19]([O:20][CH3:21])[N:14]2[N:13]=1)([CH3:5])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 59389328HCID 59389328, 화합물HCID 178420675HCID 178420675, 화합물2회

생성물 1

HCID 59389308HCID 59389308, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A 0.90 mol/L methyl magnesium bromide-tetrahydrofuran solution (0.614 mL) was added dropwise to a solution of the compound of Example 241 (55.4 mg) in THF (5 mL) at −78° C. in an argon atmosphere. The mixture was allowed to gradually warm to room temperature and was stirred for 3 hours. Subsequently, a second portion of 0.90 mol/L methyl magnesium bromide-tetrahydrofuran solution (0.614 mL) was added dropwise at −78° C. and the mixture was stirred at room temperature for another 3 hours. The reaction was then quenched by adding a saturated aqueous solution of ammonium chloride and the mixture was extracted with ethyl acetate (100 mL). The extract was washed with water and saturated brine and dried over anhydrous sodium sulfate. The dried extract was concentrated and purified by silica gel column chromatography (ethyl acetate) to afford the title compound as a pale yellow powder (14.0 mg).

후처리

  1. stirringthe mixture was stirred at room temperature for another 3 hours
  2. customThe reaction was then quenched
  3. additionby adding a saturated aqueous solution of ammonium chloride
  4. extractionthe mixture was extracted with ethyl acetate (100 mL)
  5. washThe extract was washed with water and saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. extractionThe dried extract
  8. concentrationwas concentrated
  9. custompurified by silica gel column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-32333a23298c41ebbff690c5cebaf459
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763617B2

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