関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloro-1-methylpyridinium iodide | HCID 167069 | — |
| 反応物 | 5-(3-(7-Chloroquinolin-2-ylmethoxy)phenyl)-4,6-dithianonanedioic acid | HCID 10051321 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile methylene chloride | HCID 21877088 | — |
| 生成物 | 8-Carbamyl-5-(3-(7-chloroquinolin-2-ylmethoxy)phenyl)-4,6-dithiaoctanoic acid | HCID 19930516 | — |
反応手順
The diacid (Example 3) (3.954 g, 8.04 mmoles) was dissolved in 250 mL CH2Cl2 :CH3CN 4:1. Triethylamine (2.5 mL, 2.2 equiv.) was added followed, at 0° C., by 2-chloro-1-methylpyridinium iodide (2.257 g, 1.1 equiv.). After stirring 1 hour at 0° C., ammonia was added and the mixture stirred for another hour at 10° C. Water was then added and the aqueous layer acidified to pH 5. Extraction with CH2Cl2 (2×) and EtOAc (2×) and the flash chromatography of the residue on silica with acetone:CH2Cl2 :AcOH 40:60:1 and 50:50:1 afforded the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04851409 |
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| 出典データセット | uspto-grants-1989_07 |
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| ORD ID | ord-841a44b99eeb4eb2a9bd3a5a207879ec |
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| 出典メモ | uspto-grants-1989_07 |
|---|
