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1-Naphthalenesulfonyl chloride → HCID 178453605、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Naphthalenesulfonyl chloride | HCID 66560 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | HCID 178453600 | HCID 178453600 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178453605 | HCID 178453605 | — |
反応手順
A solution of trans-(4-aminomethyl-cyclohexylmethyl)-carbamic acid tert-butyl ester (17 g) and ethyldiisopropylamine (14.41 ml) in N,N-dimethylformamide (350 ml) is cooled to 0° C. and treated with a solution of naphthalene-1-sulfonylchloride (15.9 g) in N,N-dimethylformamide (100 ml). The reaction is stirred at ambient temperature for 2 h, concentrated in vacuo. The residue is taken up in dichloromethane, washed with a 0.5 N HCl solution, a saturated aqueous sodium carbonate solution and water, dried and concentrated. Crystallization from hexanes-ethyl acetate gives trans-{4-[(naphthalene-1-sulfonylamino)-methyl]-cyclohexylmethyl}-carbamic acid tert-butyl ester as a white powder, melting at 199-200° C. Rf (A1) 0.42.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06316203B1 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-a6402fc5c94f41e5bde9ce7b6593e037 |
| 出典メモ | uspto-grants-2001_11 |