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Triethylamine → 2-Chloro-n-ethyl-n-(1-methylheptyl)-6-(trimethylsilyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Heptanamine, 1-methyl, N-ethyl | HCID 525053 | — |
| 反応物 | 2-Chloro-6-(trimethylsilyl)benzoyl chloride | HCID 15183557 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Chloro-n-ethyl-n-(1-methylheptyl)-6-(trimethylsilyl)benzamide | HCID 18630144 | 38% |
反応手順
Triethylamine (2.02 g, 20 mmol) was added to a mixture of the compound of Example b (2.47 g, 10 mmol) and N-ethyl-N-(1-methylhept-1-yl)amine (3.15 g, 20 mmol) in toluene (25 mL). The reaction was stirred 2.5 h at ambient temperature, then was partitioned between ethyl acetate and dilute citric acid. The organic phase was washed twice with sat aq NaHCO3, followed with brine, then was dried (MgSO4), concentrated, and kugelrohr distilled under vacuum. The fraction which distilled at 157° C. was collected to afford 1.16 g of the title compound as an amber oil, a 38% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06028101 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-3d764ea2e5d44b6e8f0eac8d28a98cb6 |
| 出典メモ | uspto-grants-2000_02 |