関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | methyl 1-(2,3-dichlorobenzyl)-2-(difluoromethyl)-6-morpholino-1H-benzo[d]imidazole-4-carboxylate | HCID 66976997 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 56960686 | HCID 56960686 | 46% |
反応手順
A mixture of methyl 1-(2,3-dichlorobenzyl)-2-(difluoromethyl)-6-morpholino-1H-benzo[d]imidazole-4-carboxylate (1350 mg, 2.88 mmol) and 2 N LiOH (10 mL) in THF (2.0 mL) was stirred at 45° C. for 4 h. It was filtered, the filter cake was dissolved in water (10 mL) and formic acid was added to adjust pH=3-4. Then a filtration was performed and the filter cake was dried under vacuum to give the desired product (600 mg, 46%) as a white solid. 1H NMR (300 MHz, DMSO-d6): δ ppm 3.15 (s, 4H), 3.73 (s, 4H), 5.76 (s, 2H), 6.22 (d, 1H, J=7.5 Hz), 7.20-7.60 (m, 5H), 12.98 (br s, 1H); LC-MS: m/e=456 [M+1]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08674090B2 |
|---|
| 出典データセット | uspto-grants-2014_03 |
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| ORD ID | ord-9ac779dcbfd046dea3028786d35d5a06 |
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| 出典メモ | uspto-grants-2014_03 |
|---|