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Potassium Carbonate → 4-Chloro-N-[(trimethylsilyl)methyl]benzeneethanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-(4-Chlorophenyl)ethylamine | HCID 67430 | — |
| 反応物 | Silane, (chloromethyl)trimethyl- | HCID 75361 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-Chloro-N-[(trimethylsilyl)methyl]benzeneethanamine | HCID 21301008 | 49.9% |
反応手順
The compound of formula (P11), wherein n=2 and R″ is chloro, was prepared from a mixture of chloromethyltrimethylsilane (3.7 mL, 42.8 mmol), 2-(4-chlorophenyl)ethylamine (10 g, 64.25 mmol), and K2CO3 (4 g, 28.9 mmol) in acetonitrile (80 mL). The reaction mixture was refluxed for 13 h and after cooling, the precipitate was filtered off and the filtrate concentrated under vacuum. The resulting oil was chromatographed over silica gel (CH2Cl2/MeOH/Et3N: 97/2/1) to yield the above-referenced compound as a colorless oil (5.17 g). 1H NMR (CDCl3): 7.25 (2H, d, J=8.3 Hz), 7.12 (2H, d, J=8.3 Hz), 2.7-2.9 (4H, m), 2.08 (3H, s), 0.95 (1H, br s), 0.02 (9H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06710064B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-ccecd3b1ec0946c0ae7c71dcc6b6d29d |
| 出典メモ | uspto-grants-2004_03 |