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Propionic Acid → (+/-)9-[6-(4-Methoxy-benzylamino)-pyridin-2-yl]-3-(2-methyl-pyrimidin-5-yl)-non-4-enoic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Propionic Acid | HCID 1032 | — |
| 反応物 | Triethyl orthoacetate | HCID 66221 | — |
| 反応物 | 7-[6-(4-Methoxy-benzylamino)-pyridin-2-yl]-1-(2-methyl-pyrimidin-5-yl)-hept-1-en-3-ol | HCID 69666251 | — |
| 反応物 | Hydrochloric acid brine | HCID 131718760 | — |
| 生成物 | (+/-)9-[6-(4-Methoxy-benzylamino)-pyridin-2-yl]-3-(2-methyl-pyrimidin-5-yl)-non-4-enoic acid ethyl ester | HCID 69666047 | 86% |
反応手順
A solution of the allylic alcohol 16-4 (2.3 g, 5.49 mmol) in (EtO)3CMe (10 mL) was treated with 100 uL of a 1 mL solution of (EtO)3CMe containing 10 uL of propionic acid. The yellow solution was heated at 150° for 90 minutes. The solution was cooled to room temperature and poured into 1N HCl/brine. The mixture was extracted with CHCl3, dried, concentrated, and purified on silica gel (90:5:5 CHCl3:EtOAc:MeOH) to give 2.32 g (86%) of 16-7.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07153862B2 |
| 出典データセット | uspto-grants-2006_12 |
| ORD ID | ord-098c08eb2017433d9c93bfdcfee06ce7 |
| 出典メモ | uspto-grants-2006_12 |