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Thiazolidinedione → 6-[3-(1-Adamantyl)-4-methoxyphenyl]-naphthalen-2-yl-methyl-2,4-thiazolidinedione

HRID 860545
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HRID 860545 반응식
[S:1]1[CH2:5][C:4](=[O:6])[NH:3][C:2]1=[O:7].[Li][CH2:9]CCC.[C:13]12([C:23]3[CH:24]=[C:25]([C:31]4[CH:32]=[C:33]5[C:38](=[CH:39][CH:40]=4)[CH:37]=[C:36](CI)[CH:35]=[CH:34]5)[CH:26]=[CH:27][C:28]=3[O:29][CH3:30])[CH2:22][CH:17]3[CH2:18][CH:19]([CH2:21][CH:15]([CH2:16]3)[CH2:14]1)[CH2:20]2>C1COCC1.O>[C:13]12([C:23]3[CH:24]=[C:25]([C:31]4[CH:32]=[C:33]5[C:38](=[CH:39][CH:40]=4)[CH:37]=[C:36]([CH:5]4[S:1][C:2](=[O:7])[N:3]([CH3:9])[C:4]4=[O:6])[CH:35]=[CH:34]5)[CH:26]=[CH:27][C:28]=3[O:29][CH3:30])[CH2:22][CH:17]3[CH2:18][CH:19]([CH2:21][CH:15]([CH2:16]3)[CH2:14]1)[CH2:20]2
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참가 물질

6

반응물 3

HCID 5437ThiazolidinedioneHCID 695838266-[3-(1-Adamantyl)-4-methoxyphenyl]-naphthalen-2-yl-methyliodideHCID 178418339Butyllithium

생성물 1

HCID 878990396-[3-(1-Adamantyl)-4-methoxyphenyl]-naphthalen-2-yl-methyl-2,4-thiazolidinedione수율 56%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매
2회

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온도
0 °C

실험 절차

To a stirred solution of 2,4-thiazolidinedione (0.094 g, 0.80 mmol) in 4.0 mL of anhydrous THF at −78° C. under argon was added n-BuLi (0.58 mL of 2.5 M in hexanes). After 20 minutes, the reaction mixture was allowed to warm to 0° C. for 30 minutes then cooled to −78° C. To this mixture was added 6-[3-(1-adamantyl)-4-methoxyphenyl]-naphthalen-2-yl-methyliodide (0.177 g, 0.35 mmol) in 3 mL anhydrous THF and stirred at −78° C. for 30 minutes. The reaction mixture was warmed to room temperature. After 14 hours, the reaction mixture was diluted with water and extracted with EtOAc (2×50 mL). The combined organics were washed with water (100 mL), sat. NH4Cl (100 mL), brine (100 mL), dried over anhydrous magnesium sulfate, filtered and evaporated. The residue was purified on silica gel (eluent: hexane:EtOAc 4:1) to give 0.097 g of 6-[3-(1-adamantyl)-4-methoxyphenyl]-naphthalen-2-yl-methyl-2,4-thiazolidinedione (56%), mp 251–253° C. 1H NMR (300 MHz; DMSO-d6): δ 1.80 (brs, 6H), 2.10–2.18 (m, 9H), 3.32 (dd, J=9.6 Hz, J=14.1 Hz, 1H), 3.72 (dd, J=3.6 Hz, J=14.1 Hz, 1H), 3.90 (s, 3H), 4.65 (dd, J=3.6 Hz, J=9.9 Hz, 1H), 6.99 (d, J=8.1 Hz, 1H), 7.36 (dd, J=1.5 Hz, J=8.4 Hz, 1H), 7.52 (dd, J=1.8 Hz, J=8.7 Hz, 1H), 7.57 (d, J=2.1 Hz, 1H), 7.70–7.76 (m, 2H), 7.84 (d, J=3.3 Hz, 1H), 7.87 (d, J=3.6 Hz, 1H), 7.96 (d, J=0.3 Hz, 1H), 8.13 (brs, 1H). 13C NMR (75 MHz; DMSO-d6): 38.4, 46.6, 47.4, 62.7, 65.3, 122.6, 134.0, 134.7, 135.3, 137.3, 137.6, 137.9, 138.1, 141.5, 141.8, 142.3, 144.1, 147.7, 147.8, 168.1, 181.4, 185.5.

후처리

  1. temperaturethen cooled to −78° C
  2. temperatureThe reaction mixture was warmed to room temperature
  3. waitAfter 14 hours
  4. extractionextracted with EtOAc (2×50 mL)
  5. washThe combined organics were washed with water (100 mL), sat. NH4Cl (100 mL), brine (100 mL)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was purified on silica gel (eluent: hexane:EtOAc 4:1)

출처 및 근거

ORD 기록
ord-b61002707b154dcab053bcca8fecd52c
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07153875B2

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