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Triethylamine → HCID 178491487、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | PyBOP | HCID 2724699 | — |
| 反応物 | 3-Hydroxy-3-(4-methoxyphenyl)propanoic acid | HCID 14927307 | — |
| 反応物 | HCID 178474312 | HCID 178474312 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178491487 | HCID 178491487 | 77.4% |
反応手順
A mixture of 3-hydroxy-3-(4-methoxyphenyl)propanoic acid (13.7 mg, 0.07 mmol), (Z)-tert-butyl (4-acetamido-3,5-dichlorobenzylamino)(amino)-methylenecarbamate (26.3 mg), PyBop (36.4 mg), and triethylamine (0.01 mL) in dichloromethane (0.35 mL) was stirred at room temperature for 12 h. The crude reaction mixture was purified directly by preparative TLC eluting with 30% ethyl acetate/70% hexanes to give the title compound as a clear sticky oil (30 mg, 77% yield). 1H NMR (400 MHz, CDCl3) δ 1.48 (m, 9 H) 2.21 (s, 3 H) 2.70 (m, 2 H) 3.78 (m, 3 H) 4.55 (m, 2 H) 4.95 (m, 1 H) 6.80-7.00 (m, 3 H) 7.24-7.38 (m, 4 H), 9.10 (m, 1 H), 12.30 (m, 1 H). HPLC retention time: 2.493 min (method A). MS (ESI) (M+H)+ 553.08.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07390925B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-e2bed52f21754bca906fd61d26a1a75a |
| 出典メモ | uspto-grants-2008_06 |