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Trityl chloride → Phenyl [1-methyl-5-(tritylamino)pyrazol-4-yl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Heptane | HCID 8900 | — |
| 反応物 | 5-Amino-1-methyl-4-phenoxycarbonylaminopyrazole | HCID 21904460 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Phenyl [1-methyl-5-(tritylamino)pyrazol-4-yl]carbamate | HCID 21904567 | 80.7% |
反応手順
To a suspension of 5-amino-1-methyl-4-phenoxycarbonylaminopyrazole (153.8 g) in tetrahydrofuran (1 L) were added triethylamine (67 g) and triphenylmethyl chloride (185 g) at room temperature. The mixture was stirred for 6.5 hours. To the reaction mixture was added heptane (2.6 L), and the mixture was stirred for 1 hour. The precipitated solid was collected by filtration and washed with heptane-diisopropyl ether (1:1). The crude solid was suspended in water (3 L), and the suspension was stirred for 1 hour. The solid was collected by filtration and dried to give 1-methyl-4-phenoxycarbonylamino-5-triphenylmethylaminopyrazole (253.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129232B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-02c9f3e376fb4ab6bb6c7b51f778d54c |
| 出典メモ | uspto-grants-2006_10 |