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HRID 18749作成日：2026年10月23日
3,4-Difluorobenzylamine → tert-butyl (3aR,7aS)-2-[(3,4-difluorophenyl)methylamino]-3a,4,5,6,7,7a-hexahydrobenzimidazole-1-carboxylate
https://huagongshe.com/ja/reaction/18749
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Difluorobenzylamine | HCID 123572 | — |
| 反応物 | cis-3a,4,5,6,7,7a-Hexahydro-2-methylthio-benzimidazole-1-carboxylic Acid, Tert-Butyl Ester | HCID 86596330 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | tert-butyl (3aR,7aS)-2-[(3,4-difluorophenyl)methylamino]-3a,4,5,6,7,7a-hexahydrobenzimidazole-1-carboxylate | HCID 68568451 | 99.8% |
反応手順
A mixture of intermediate 76 (200 mg, 0.740 mmol), 3,4-difluorobenzylamine (0.5 mL, 4.2 mmol) is heated at 100° C. (reaction block) overnight. The reaction mixture is cooled to RT. The reaction mixture is diluted with dichloromethane, washed with 0.1N HCl, and brine. The solvent is evaporated, and the residue triturated with EtOAc, and the insoluble material filtered to give 270 mg of the product 195. 1H NMR (CDCl3) δ 8.60 (s, 1 H), 7.40-7.10 (m, 3 H), 5.15-4.90 (m, 2 H), 4.30-4.10 (m, 2 H), 2.70-2.55 (m, 1 H), 2.20-2.05 (m, 1 H), 1.85-1.10 (m, 15 H); MS: m/z 366 (M++1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741493B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-e28b7ea43af34b80a87b9ebc21e193e0 |
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| 出典メモ | uspto-grants-2010_06 |
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