関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Bromo-4-chlorothieno[2,3-d]pyrimidine | HCID 45480299 | — |
| 反応物 | 4-(2-Pyrrolidin-1-ylethoxymethyl)piperidine | HCID 62338872 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-Bromo-4-[4-(2-pyrrolidin-1-ylethoxymethyl)-1-piperidyl]thieno[2,3-d]pyrimidine | HCID 89579634 | 93.4% |
反応手順
5-Bromo-4-chlorothieno[2,3-d]pyrimidine (828 mg 3.33 mmol) in dry acetonitrile (13 mL) was treated with 4-(2-pyrrolidin-1-ylethoxymethyl)piperidine (1.057 g, 5.0 mmol,) and potassium carbonate (687 mg, 5.0 mmol) and heated at 110° C. for 30 min in a microwave. The reaction was then poured into ethyl acetate (50 mL) and water (30 mL) and the ethyl acetate layer separated, dried over sodium sulphate and concentrated in vacuum to give 5-bromo-4-[4-(2-pyrrolidin-1-ylethoxymethyl)-1-piperidyl]thieno[2,3-d]pyrimidine (1.322 g, 3.11 mmol, 93%). LCMS RT=2.91 min. M+1=427.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09290511B2 |
|---|
| 出典データセット | uspto-grants-2016_03 |
|---|
| ORD ID | ord-a26ce6502f2e45e6aea926548a44d7cb |
|---|
| 出典メモ | uspto-grants-2016_03 |
|---|
