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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Potassium Carbonate → HCID 57699826, 화합물

HRID 1011039
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HRID 1011039 반응식
FC(F)(F)C(O)=O.[CH3:8][CH:9]([O:11][CH2:12][CH2:13][O:14][C:15]1[N:23]=[C:22]2[C:18]([N:19]=[C:20]([O:24][CH3:25])[NH:21]2)=[C:17]([NH2:26])[N:16]=1)[CH3:10].C(=O)([O-])[O-].[K+].[K+].CS(O[CH2:38][CH:39]1[CH2:44][CH2:43][O:42][CH2:41][CH2:40]1)(=O)=O>CN(C)C=O.C(OCC)(=O)C>[CH3:10][CH:9]([O:11][CH2:12][CH2:13][O:14][C:15]1[N:23]=[C:22]2[C:18]([N:19]=[C:20]([O:24][CH3:25])[N:21]2[CH2:38][CH:39]2[CH2:44][CH2:43][O:42][CH2:41][CH2:40]2)=[C:17]([NH2:26])[N:16]=1)[CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 15166436Oxan-4-ylmethyl methanesulfonateHCID 178493998HCID 178493998, 화합물

생성물 1

HCID 57699826HCID 57699826, 화합물수율 112.7%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate
용매

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온도
60 °C

실험 절차

To a solution of 2-({2-[(1-methylethyl)oxy]ethyl}oxy)-8-(methoxy)-9H-purin-6-amine trifluoroacetate salt (400 mg) in dry N,N-dimethylformamide (6.4 ml) was added potassium carbonate (579 mg). The reaction was stirred at 60° C. for 1.5 hours. The reaction was cooled and tetrahydro-2H-pyran-4-ylmethyl methanesulfonate (224 mg) was added. The reaction was stirred at 90° C. for 4 hours. The reaction was cooled and taken up in ethyl acetate and washed twice with water. The organic layer was separated, dried over magnesium sulphate, filtered and concentrated in vacuo to yield a yellow oil (432 mg). The product was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluant (20-50%) to afford the title compound as a clear viscous oil (166 mg).

후처리

  1. temperatureThe reaction was cooled
  2. stirringThe reaction was stirred at 90° C. for 4 hours
  3. temperatureThe reaction was cooled
  4. washwashed twice with water
  5. customThe organic layer was separated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f36145ade31a4edea4995b80fa408bfc
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977344B2

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