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Trimethyltin chloride → 1-Methyl-5-(trimethylstannyl)-1H-1,2,3-triazole

HRID 1888466
ノート
印刷プレビュー

反応式

HRID 1888466 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[N:3]1.C([Li])CCC.Cl[Sn:13]([CH3:16])([CH3:15])[CH3:14]>O1CCCC1>[CH3:1][N:2]1[C:6]([Sn:13]([CH3:16])([CH3:15])[CH3:14])=[CH:5][N:4]=[N:3]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

5

反応物 3

HCID 14016Trimethyltin chlorideHCID 1401191-Methyl-1H-1,2,3-triazoleHCID 178418339Butyllithium

生成物 1

HCID 582665311-Methyl-5-(trimethylstannyl)-1H-1,2,3-triazole収率 94.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-30 °C

実験手順

To a stirred solution of 1-methyl-1H-1,2,3-triazole (0.5 g, 6.0 mmol) in anhydrous tetrahydrofuran (50 mL) at −78° C. under an atmosphere of nitrogen was added n-butyllithium (2.5M solution in hexanes, 2.6 mL, 6.6 mmol) dropwise over ten minutes. On complete addition the reaction was allowed to warm to −30° C. and stirred for 2 h. A solution of chlorotrimethylstannane (1.3 g, 6.6 mmol) in tetrahydrofuran (2 mL) was added dropwise over 10 minutes then the reaction mixture was allowed to warm to room temperature over 2 h. The reaction was quenched by the addition of saturated ammonium chloride solution (5 mL) then diluted with water (20 mL). The solvent was evaporated in vacuo and the aqueous phase extracted with ethyl acetate (2×30 mL). The combined organic layer was dried over sodium sulfate, filtered and concentrated to afford a pale yellow oil (1.4 g, 90%). 1H NMR (DMSO-D6, 400 MHz): 7.61 (s, 1H), 4.04 (s, 3H), 0.40 (s, 9H).

後処理

  1. additionOn complete addition the reaction
  2. temperatureto warm to room temperature over 2 h
  3. customThe reaction was quenched by the addition of saturated ammonium chloride solution (5 mL)
  4. additionthen diluted with water (20 mL)
  5. customThe solvent was evaporated in vacuo
  6. extractionthe aqueous phase extracted with ethyl acetate (2×30 mL)
  7. dry with materialThe combined organic layer was dried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-4ed0f2f38bc84b22967e988375737a61
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501765B2

反応ノート

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