関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Dichloroisoquinoline | HCID 298625 | — |
| 反応物 | HCID 15676964 | HCID 15676964 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Isobutyl 1-(3-chloroisoquinolin-1-yl)piperidin-4-ylcarbamate | HCID 59216558 | — |
反応手順
A mixture of 1,3-dichloroisoquinoline (0.16 g, 0.78 mmol), isobutyl piperidin-4-ylcarbamate (0.16 g, 0.78 mmol), Et3N (0.11 mL, 0.78 mmol), and DMF (0.5 mL) was sealed in a microwave vessel and heated by microwave irradiation at 160° C. for three minutes. The reaction was cooled to room temperature, diluted with water, and extracted with CH2Cl2. The combined extracts were washed with water, dried over Na2SO4, and concentrated under reduced pressure to yield isobutyl 1-(3-chloroisoquinolin-1-yl)piperidin-4-ylcarbamate. LC/MS: m/z 362.2 (M+H)+ at 3.98 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07683066B2 |
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| 出典データセット | uspto-grants-2010_03 |
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| ORD ID | ord-abb0c9b9cf6945f895b07e78ffd1088c |
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| 出典メモ | uspto-grants-2010_03 |
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