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4-Methylmorpholine → HCID 18680124、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | N,O-Dimethylhydroxylamine | HCID 14232 | — |
| 反応物 | 2-(tert-Butoxycarbonyl)-1,2,3,4-tetrahydroisoquinoline-6-carboxylic acid | HCID 11357887 | — |
| 反応物 | 4-(4,6-Dimethoxy[1.3.5]triazin-2-yl)-4-methylmorpholinium chloride hydrate | HCID 23149411 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 18680124 | HCID 18680124 | — |
反応手順
To 2.00 g (7.21 mmol) 3,4-dihydro-1H-isoquinoline-2,6-dicarboxylic acid 2-tert-butyl ester in 70 mL MeOH is added at RT 844 mg (8.65 mmol) O,N-dimethyl-hydroxylamine and 1.59 mL (14.4 mmol) 4-methyl-morpholine. The mixture is stirred at RT and then 2.10 g (7.57 mmol) 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methyl-morpholin-4-ium chloride hydrate is added and the mixture is stirred overnight at RT. The residue is directly purified via reverse HPLC chromatography (Waters XBridge, C18; water (0.3% NH4OH)/acetonitrile (0.3% NH4OH) 90:10 to 10:90).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08067590B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-5dfed17fa6414ec0a2af8c145c82fe6d |
| 出典メモ | uspto-grants-2011_11 |