関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | HCID 19076509 | HCID 19076509 | — |
| 反応物 | 4-(2-Methylbutan-2-yl)benzene-1-sulfonyl chloride | HCID 22281976 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 19076484 | HCID 19076484 | 29.7% |
反応手順
A solution of 1 g of 5-chloro-3-(2-chlorophenyl)-1,3-dihydro-3-[[2-(morpholin-4-yl)ethyl]amino]indol-2-one in 10 ml of DMF is cooled to 0° C. under an argon atmosphere and 0.108 g of sodium hydride as a 60% dispersion in oil is added. After stirring for 30 minutes, 0.607 g of 4-(1,1-dimethylpropyl)benzenesulfonyl chloride is added and the reaction mixture is stirred for 2 hours, the temperature being allowed to rise to RT. It is poured into water and extracted with AcOEt, the organic phase is washed with water and dried over sodium sulfate and the solvent is evaporated off under vacuum. The residue is chromatographed on silica using a DCM/AcOEt mixture (80/20; v/v) as the eluent to give 0.45 g of the expected product after crystallization from a DCM/iso ether mixture. M.p.=147° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05594023 |
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| 出典データセット | uspto-grants-1997_01 |
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| ORD ID | ord-97821cec90dd424ebf695172d0a1d62e |
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| 出典メモ | uspto-grants-1997_01 |
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