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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1-[4,6-Bis(1,1-dimethylethyl)-5-hydroxy-2-pyrimidinyl]-6-trimethylsilyl-5-hexyn-1-one → 1-[4,6-Bis(1,1-dimethylethyl)-5-hydroxy-2-pyrimidinyl]-5-hexyn-1-one

HRID 2082032
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인쇄 미리보기

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HRID 2082032 반응식
[CH3:1][C:2]([C:5]1[C:10]([OH:11])=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[N:8]=[C:7]([C:16](=[O:26])[CH2:17][CH2:18][CH2:19][C:20]#[C:21][Si](C)(C)C)[N:6]=1)([CH3:4])[CH3:3].O.O.[F-].[K+]>CN(C)C=O>[CH3:4][C:2]([C:5]1[C:10]([OH:11])=[C:9]([C:12]([CH3:13])([CH3:14])[CH3:15])[N:8]=[C:7]([C:16](=[O:26])[CH2:17][CH2:18][CH2:19][C:20]#[CH:21])[N:6]=1)([CH3:1])[CH3:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 104520651-[4,6-Bis(1,1-dimethylethyl)-5-hydroxy-2-pyrimidinyl]-6-trimethylsilyl-5-hexyn-1-oneHCID 23708904Potassium fluoride dihydrate

생성물 1

HCID 104026731-[4,6-Bis(1,1-dimethylethyl)-5-hydroxy-2-pyrimidinyl]-5-hexyn-1-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

A mixture of 1-[4,6-bis(1,1-dimethylethyl)-5-hydroxypyrimidin-2-yl]-6-trimethylsilyl-5-hexyn-1-one (0.87 g, 2.3 mmol), Example 8, and potassium fluoride dihydrate (0.91 g, 9.7 mmol) in N,N-dimethylformamide (12 mL) is warmed to 50° C. After stirring for 47 hours at 50° C., the solvent is removed under vacuum and the organic residue is diluted with water. This mixture is extracted with ethyl acetate and the combined extracts are washed with saturated aqueous ammonium chloride solution and brine. The organic is concentrated under vacuum and the organic residue purified by flash chromatorgraphy (SiO2, 20% ethyl acetate (hexane) followed by recrystallization from methanol and water to give 0.48 g (68%) of the title compound), mp 64°-66° C.

후처리

  1. customthe solvent is removed under vacuum
  2. additionthe organic residue is diluted with water
  3. extractionThis mixture is extracted with ethyl acetate
  4. washthe combined extracts are washed with saturated aqueous ammonium chloride solution and brine
  5. concentrationThe organic is concentrated under vacuum
  6. customthe organic residue purified by flash chromatorgraphy (SiO2, 20% ethyl acetate (hexane) followed by recrystallization from methanol and water to give 0.48 g (68%) of the title compound), mp 64°-66° C.

출처 및 근거

ORD 기록
ord-0d36db042726453b98e1b22d12424a22
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05187175

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