関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzenesulfonyl chloride | HCID 7369 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-((Trimethylsilyl)oxy)-N-(2-((trimethylsilyl)oxy)ethyl)ethanamine | HCID 30324 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | N,N-bis(2-trimethylsilyloxyethyl)benzenesulfonamide | HCID 18935901 | 88% |
反応手順
To a mixture of 4.97 g of bis(2-trimethylsilyloxylethyl)amine, 3.03 g of triethylamine and 50 ml of benzene, 3.21 g of benzenesulfonyl chloride was added at 0° C. under stirring. After the addition, the mixture was taken out of the cooling bath and stirred further for 2 hours. The reaction mixture was filtered, mixture was taken out of the cooling bath and stirred further for 2 hours. The reaction mixture was filtered, and the filtrate was subjected to vacuum distillation. The residue was passed through a silica gel column with the eluent varying from benzene to benzen-acetic acid (9:1). As a result, 6.23 g of the title compound was obtained as a colorless oily substance. NMRδ: 7.83 (2H,d,J=8.0 Hz),7.52 (3H,m), 3.72, 3.31 (each 4H,t,J=6.5 Hz), 0.09 (18H,s)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05730953 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-ee33145d3712452584d543409e62c64a |
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| 出典メモ | uspto-grants-1998_03 |
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