関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzophenone | HCID 3102 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Glycine tert-butyl ester | HCID 151417 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(Diphenylmethylene)glycine tert-butyl ester | HCID 688171 | 48.8% |
反応手順
A solution of t-butyl 2-aminoacetate (113.7 g, 866.8 mmol, 1.0 equiv) in toluene (1000 mL) was combined with benzophenone (157.9 g, 866.5 mmol, 1.0 equiv) and 4-methylbenzenesulfonic acid (14.9 g, 86.5 mmol, 0.1 equiv). The resulting solution was heated to reflux overnight. The mixture was then concentrated in vacuo to 600 mL. The mixture was cooled to 15° C. with a water/ice bath. The product precipitated and the solids were collected by filtration. The solids was washed with petroleum ether (5×150 mL) to yield t-butyl 2-(diphenylmethyleneamino)acetate (125 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08372984B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-6ecd3f1a47434f90bf24de5f5ac70dd4 |
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| 出典メモ | uspto-grants-2013_02 |
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