関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Dipotassium 2,3-dihydroxybutanedioate | HCID 6100505 | — |
| 反応物 | N-Ethyl-n-heptyl-4-(4-(methylsulfonamido)phenyl)-4-oxobutanamide | HCID 14891420 | — |
| 反応物 | N-(4-Acetyl-2-methylphenyl)methanesulfonamide | HCID 19873430 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ibutilide | HCID 60753 | — |
反応手順
A stirred suspension of lithium aluminum hydride (0.86 g, 0.0227 mol) in dry tetrahydrofuran (30 ml) under nitrogen is cooled to 0° to -5° C. and treated dropwise during 25 minutes with a solution of N-ethyl-N-heptyl-γ-oxo-4-[(methylsulfonyl)amino]benzenebutanamide as prepared in Preparation 3 (3.0 g, 0.00757 mole) in THF (30 ml). After 2.5 hours this mixture is treated dropwise with a saturated solution of sodium, potassium tartrate (10 ml) and then with ethyl acetate. The mixture is filtered and the solid is extracted with ethyl acetate. The organic solutions are dried (MgSO4) and concentrated; the residual product is combined to give 2.10 g of N-[4-[4-(ethylheptylamino)-1-hydroxybutyl]phenyl]methanesulfonamide. By NMR this material is the same as an authentic sample obtained from another reaction and purified by silica gel chromatography with 0.5% NH4OH-6% MeOH--CH2Cl2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05155268 |
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| 出典データセット | uspto-grants-1992_10 |
|---|
| ORD ID | ord-fb0211ba58e54922a4a3be53e4193a78 |
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| 出典メモ | uspto-grants-1992_10 |
|---|
