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Tributyltin Chloride → HCID 68159442、化合物

HRID 2360542
ノート
印刷プレビュー

反応式

HRID 2360542 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[S:10][CH:9]=[N:8][CH:7]=1.C([Li])CCC.C([Sn](Cl)(CCCC)CCCC)CCC.C1(C)C(C([O:38][C@@H:39]2[C@@H:43]([CH2:44][O:45]C(C3C(C)=CC=CC=3)=O)[O:42][C@@H:41]([N:55]3[C:59]4=[N:60][CH:61]=[CH:62][C:63](I)=[C:58]4[CH:57]=[CH:56]3)[CH2:40]2)=O)=CC=CC=1>C(OCC)C.CN(C=O)C>[C@@H:41]1([N:55]2[C:59]3=[N:60][CH:61]=[CH:62][C:63]([C:9]4[S:10][C:6]([C:2]5[S:1][CH:5]=[CH:4][CH:3]=5)=[CH:7][N:8]=4)=[C:58]3[CH:57]=[CH:56]2)[O:42][C@H:43]([CH2:44][OH:45])[C@@H:39]([OH:38])[CH2:40]1
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

7

反応物 4

HCID 15096Tributyltin ChlorideHCID 11217456Thiazole, 5-(2-thienyl)-HCID 131731282HCID 131731282、化合物HCID 178418339Butyllithium

生成物 1

HCID 68159442HCID 68159442、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
-78 °C

実験手順

A solution of 5-(2-thienyl)thiazole (0.4 mmol) in diethyl ether was cooled to −78° C., and n-butyllithium (0.4 mmol, 1.57 M solution in hexane) was added thereto, followed by stirring at −78° C. for 30 min. Furthermore, tributylstannyl chloride was added thereto, followed by stirring at room temperature for 30 min. The reaction solution was separated between ethyl acetate and water. The organic layer was washed with saturated brine and concentrated, and 1-[2-deoxy-3,5-di-O-(toluoyl)-β-D-ribofuranosyl]-4-iodo-pyrrolo[2,3-b]pyridine (120 mg, 0.2 mmol), chlorobistriphenylphosphine palladium (5% mol), and DMF (2 mL) were added thereto, followed by stirring at 100° C. for 1 hr. The reaction solution was separated between ethyl acetate and water, and the organic layer was washed with saturated brine and water, dried over anhydrous sodium sulfate, and concentrated. After purification with a silica gel column and addition of sodium methoxide (1.6 mL), the resulting mixture was stirred at room temperature for 30 min. dDvas nucleoside (34 mg) was purified with a silica gel column and by HPLC.

後処理

  1. stirringby stirring at room temperature for 30 min
  2. customThe reaction solution was separated between ethyl acetate and water
  3. washThe organic layer was washed with saturated brine
  4. concentrationconcentrated
  5. stirringby stirring at 100° C. for 1 hr
  6. customThe reaction solution was separated between ethyl acetate and water
  7. washthe organic layer was washed with saturated brine and water
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. customAfter purification
  11. additionwith a silica gel column and addition of sodium methoxide (1.6 mL)
  12. stirringthe resulting mixture was stirred at room temperature for 30 min. dDvas nucleoside (34 mg)
  13. customwas purified with a silica gel column and by HPLC

出典と根拠

ORDレコード
ord-e9c2cd1ce0e3417bb6057d65505e55f5
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08686130B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート