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Lithium Hexamethyldisilazide → 1-chloro-N-(2,4-dimethoxybenzyl)-N-(thiazol-2-yl)isoquinoline-6-sulfonamide

HRID 1473325
ノート
印刷プレビュー

反応式

HRID 1473325 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]([N-][Si](C)(C)C)(C)C.[Li+].[Cl:28][C:29]1[C:38]2[C:33](=[CH:34][C:35]([S:39](Cl)(=[O:41])=[O:40])=[CH:36][CH:37]=2)[CH:32]=[CH:31][N:30]=1>C1COCC1>[Cl:28][C:29]1[C:38]2[C:33](=[CH:34][C:35]([S:39]([N:6]([CH2:5][C:4]3[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:3]=3[O:2][CH3:1])[C:7]3[S:8][CH:9]=[CH:10][N:11]=3)(=[O:41])=[O:40])=[CH:36][CH:37]=2)[CH:32]=[CH:31][N:30]=1
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 HexamethyldisilazideHCID 49931979N-(2,4-dimethoxybenzyl)thiazol-2-amineHCID 861938101-Chloroisoquinoline-6-sulfonyl chloride

生成物 1

HCID 866873781-chloro-N-(2,4-dimethoxybenzyl)-N-(thiazol-2-yl)isoquinoline-6-sulfonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of N-(2,4-dimethoxybenzyl)thiazol-2-amine (0.546 g, 2.182 mmol) in THF (7 mL) was cooled in a dry ice-acetone bath for 5 minutes. Lithium bis(trimethylsilyl)amide (1M in THF) (2.381 ml, 2.381 mmol) was added dropwise, then the flask was removed from the cooling bath for 5 min. The flask was again cooled into a dry ice-acetone bath for 20 min, resulting in the formation of a thick slurry. A suspension of 1-chloroisoquinoline-6-sulfonyl chloride (0.520 g, 1.984 mmol) in THF (5 mL) was added dropwise, then the cooling bath was removed. The reaction was stirred for one hour. The reaction was quenched with saturated ammonium chloride solution, diluted with ethyl acetate and washed with water. The aqueous layer was extracted with ethyl acetate, and the combined organic layers were dried with sodium sulfate, filtered, and concentrated. The filtrate was purified by silica gel chromatography on a 40 g silica column with 0 to 30% EtOAc/Heptane. The product containing fractions were combined and concentrated to afford a white solid. The solid was triturated with methanol and stirred for five minutes. The solution was filtered and the solids were washed with methanol. The solids were dried under a vacuum to afford 1-chloro-N-(2,4-dimethoxybenzyl)-N-(thiazol-2-yl)isoquinoline-6-sulfonamide as a white solid. m/z (ESI) 498.1 (M+H)+.

後処理

  1. customthe flask was removed from the cooling bath for 5 min
  2. temperatureThe flask was again cooled into a dry ice-acetone bath for 20 min
  3. customresulting in the formation of a thick slurry
  4. additionwas added dropwise
  5. customthe cooling bath was removed
  6. customThe reaction was quenched with saturated ammonium chloride solution
  7. additiondiluted with ethyl acetate
  8. washwashed with water
  9. extractionThe aqueous layer was extracted with ethyl acetate
  10. dry with materialthe combined organic layers were dried with sodium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated
  13. customThe filtrate was purified by silica gel chromatography on a 40 g silica column with 0 to 30% EtOAc/Heptane
  14. additionThe product containing fractions
  15. concentrationconcentrated
  16. customto afford a white solid
  17. customThe solid was triturated with methanol
  18. stirringstirred for five minutes
  19. filtrationThe solution was filtered
  20. washthe solids were washed with methanol
  21. customThe solids were dried under a vacuum

出典と根拠

ORDレコード
ord-6fc7d2a7138d421fbd4d3ecf523c8396
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09012443B2

反応ノート

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