Sodium Methoxide → 2-[(2-Cyclopropylethyl)oxy]-8-methoxy-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine

HRID 1011057노트

반응식

HRID 1011057 반응식
Br[C:2]1[N:3]([CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][O:19]2)[C:4]2[C:9]([N:10]=1)=[C:8]([NH2:11])[N:7]=[C:6]([O:12][CH2:13][CH2:14][CH:15]1[CH2:17][CH2:16]1)[N:5]=2.[CH3:24][O-:25].[Na+]>CO>[CH:15]1([CH2:14][CH2:13][O:12][C:6]2[N:5]=[C:4]3[C:9]([N:10]=[C:2]([O:25][CH3:24])[N:3]3[CH:18]3[CH2:23][CH2:22][CH2:21][CH2:20][O:19]3)=[C:8]([NH2:11])[N:7]=2)[CH2:17][CH2:16]1

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 576996678-Bromo-2-[(2-cyclopropylethyl)oxy]-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine

생성물 1

HCID 576996292-[(2-Cyclopropylethyl)oxy]-8-methoxy-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A stirring suspension of 8-bromo-2-[(2-cyclopropylethyl)oxy]-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (7.96 g) in methanol (80 ml) was treated with 25 wt % sodium methoxide in methanol (14.29 ml) and refluxed under nitrogen for 3.5 h. After allowing to cool over 16 h the solvent was evaporated and the residue treated with saturated ammonium chloride and extracted twice with ethyl acetate. The combined extracts were washed with brine, dried by passing through a hydrophobic frit and evaporated to give the title compound as a brown solid, yield 6.49 gm.

후처리

  1. temperaturerefluxed under nitrogen for 3.5 h
  2. temperatureto cool over 16 h the solvent
  3. customwas evaporated
  4. additionthe residue treated with saturated ammonium chloride
  5. extractionextracted twice with ethyl acetate
  6. washThe combined extracts were washed with brine
  7. customdried
  8. customevaporated

출처 및 근거

ORD 기록
ord-34e85deba9cd4ee19bdc411a28d22528
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977344B2

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