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Carbon Dioxide → HCID 22257999, 화합물

HRID 1611022
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HRID 1611022 반응식
C([Li])CCC.C(NC(C)C)(C)C.[CH3:13][N:14]1[C:19](=[O:20])[C:18]2[CH:21]=[C:22]([CH2:24][C:25]3[C:34]4[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=4)[CH:28]=[CH:27][CH:26]=3)[S:23][C:17]=2[N:16]([CH2:35][CH:36]([CH3:38])[CH3:37])[C:15]1=[O:39].[C:40](=[O:42])=[O:41].[OH-].[Na+]>O1CCCC1>[CH3:13][N:14]1[C:19](=[O:20])[C:18]2[C:21]([C:40]([OH:42])=[O:41])=[C:22]([CH2:24][C:25]3[C:34]4[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=4)[CH:28]=[CH:27][CH:26]=3)[S:23][C:17]=2[N:16]([CH2:35][CH:36]([CH3:37])[CH3:38])[C:15]1=[O:39]
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참가 물질

7

반응물 5

HCID 280Carbon DioxideHCID 7912DiisopropylamineHCID 14798Sodium HydroxideHCID 5282538HCID 5282538, 화합물HCID 178418339Butyllithium

생성물 1

HCID 22257999HCID 22257999, 화합물

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

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온도
-78 °C

실험 절차

n-Butyllithium (2.0M solution in hexanes, 1.90 ml) was added dropwise to a solution of diisopropylamine (0.069 ml) in anhydrous tetrahydrofuran (30 ml) at 0° C., under nitrogen. The solution was stirred for 5 minutes then cooled to −78° C. and a solution of 3-methyl-1-(2-methylpropyl)-6-(1-naphthalenylmethyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (1.50 g) in anhydrous tetrahydrofuran (15 ml) was added dropwise. After 15 minutes, the flask was transferred to a sealed bomb containing carbon dioxide pellets (2 g) and heated to 50° C. for 18 hours. The reaction mixture was cooled to room temperature then added to aqueous sodium hydroxide solution (0.25M, 75 ml) and washed with ether (2×75 ml). The aqueous layer was acidified with concentrated hydrochloric acid and extracted with ether (2×75 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by column chromatography over silica, eluting with isohexane:ethyl acetate (3:1) containing 1% acetic acid, to give the subtitle compound (0.337 g) as a solid.

후처리

  1. waitAfter 15 minutes
  2. temperatureheated to 50° C. for 18 hours
  3. temperatureThe reaction mixture was cooled to room temperature
  4. washwashed with ether (2×75 ml)
  5. extractionextracted with ether (2×75 ml)
  6. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customevaporated under reduced pressure
  9. customThe residue was purified by column chromatography over silica
  10. washeluting with isohexane:ethyl acetate (3:1)
  11. additioncontaining 1% acetic acid

출처 및 근거

ORD 기록
ord-e7124a9eb24f4a4da3b894201f0e84b4
출처 데이터셋
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06984644B2

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