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

HRID 860545
ノート
印刷プレビュー

反応式

HRID 860545 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b61002707b154dcab053bcca8fecd52c
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07153875B2

反応ノート

読み込み中…

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