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Lithium hexamethyldisilazane → N-(2,4-dimethoxybenzyl)-5-iodo-N-(thiazol-2-yl)pyridine-2-sulfonamide

HRID 1644664
ノート
印刷プレビュー

反応式

HRID 1644664 の反応式
[CH3:1][O:2][C:3]1[CH:15]=[C:14]([O:16][CH3:17])[CH:13]=[CH:12][C:4]=1[CH2:5][NH:6][C:7]1[S:8][CH:9]=[CH:10][N:11]=1.C[Si](C)(C)[N-][Si](C)(C)C.[Li+].[I:28][C:29]1[CH:30]=[CH:31][C:32]([S:35](Cl)(=[O:37])=[O:36])=[N:33][CH:34]=1>O1CCCC1>[CH3:1][O:2][C:3]1[CH:15]=[C:14]([O:16][CH3:17])[CH:13]=[CH:12][C:4]=1[CH2:5][N:6]([C:7]1[S:8][CH:9]=[CH:10][N:11]=1)[S:35]([C:32]1[CH:31]=[CH:30][C:29]([I:28])=[CH:34][N:33]=1)(=[O:37])=[O:36]
参加物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 2733832Lithium hexamethyldisilazaneHCID 49931979N-(2,4-dimethoxybenzyl)thiazol-2-amineHCID 575511815-Iodopyridine-2-sulfonyl chloride

生成物 1

HCID 57551263N-(2,4-dimethoxybenzyl)-5-iodo-N-(thiazol-2-yl)pyridine-2-sulfonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

(2,4-Dimethoxy-benzyl)-thiazol-2-yl-amine (0.453 g, 1.81 mmol) was dissolved in Tetrahydrofuran (5 mL, 70 mmol) and cooled in an ice bath. 1.0 M of Lithium hexamethyldisilazide in Tetrahydrofuran (2.0 mL) was added dropwise to the reaction. After addition was complete, the reaction mixture was warmed to ambient temperature. After 30 min, the reaction was cooled to at 0° C. and a solution of 5-Iodo-pyridine-2-sulfonyl chloride (0.50 g, 1.6 mmol) in Tetrahydrofuran (4 mL, 50 mmol) was added dropwise. The reaction mixture was stirred 4 h then quenched with saturated aqueous ammonium chloride. The reaction mixture was concentrated in vacuo. The residue was taken up in ethyl acetate and additional saturated aqueous ammonium chloride was added. The layers were separated, and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered through celite, and concentrated in vacuo. The residue was purified on the ISCO twice (hexanes to ethyl acetate) to afford the product as a yellow solid.

後処理

  1. temperaturecooled in an ice bath
  2. additionAfter addition
  3. temperaturethe reaction was cooled to at 0° C.
  4. customthen quenched with saturated aqueous ammonium chloride
  5. concentrationThe reaction mixture was concentrated in vacuo
  6. additionadditional saturated aqueous ammonium chloride was added
  7. customThe layers were separated
  8. extractionthe aqueous layer was extracted with ethyl acetate
  9. washThe combined organic layers were washed with brine
  10. dry with materialdried over sodium sulfate
  11. filtrationfiltered through celite
  12. concentrationconcentrated in vacuo
  13. customThe residue was purified on the ISCO twice (hexanes to ethyl acetate)

出典と根拠

ORDレコード
ord-a6469b1d0b7941f0965c1f296f8df01f
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08124610B2

反応ノート

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