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4-(5-Chloro-2-methoxy-phenyl)-4-methoxy-piperidine-1-carboxylic acid tert-butyl ester → Hydrochloric Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-(5-Chloro-2-methoxy-phenyl)-4-methoxy-piperidine-1-carboxylic acid tert-butyl ester | HCID 58772528 | — |
| 溶媒 | Hydrochloride methanol | HCID 21893726 | — |
| 生成物 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 4-(5-Chloro-2-methoxyphenyl)-4-methoxypiperidine | HCID 58772297 | — |
反応手順
A solution of 4-(5-chloro-2-methoxy-phenyl)-4-methoxy-piperidine-1-carboxylic acid tert-butyl ester 5c (3.8 g, crude from last step) in methanol/HCl (2 M, 50 mL) was stirred at room temperature for 4 h, then the mixture was concentrated to half of volume under 40° C. and then ether was added. The precipitated was filtered and washed with ether to obtain 4-(5-chloro-2-methoxyphenyl)-4-methoxypiperidine 5d as its HCl salt. 1H NMR (DMSO-d6): δ 8.95 (b, 2H), 7.37-7.34 (q, J1=8.8 Hz, J2=8.8 Hz, 1H), 7.21-7.20 (d, J=2.8 Hz, 1H), 7.09-7.07 (d, J=8.8 Hz, 1H), 3.78 (s, 3H), 3.16-3.13 (m, 2H), 3.13-2.98 (m, 5H), 2.35-2.28 (m, 2H), 2.19-2.16 (m, 2H). ESI-MS m/z 256.8.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07880007B2 |
| 出典データセット | uspto-grants-2011_02 |
| ORD ID | ord-38d2ce59f83649bfb3dad518bd2060c6 |
| 出典メモ | uspto-grants-2011_02 |