関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 反応物 | Z-Phg-OH | HCID 819214 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 36690768 | HCID 36690768 | 68.7% |
反応手順
27.6 g (97 mmoles) of Z-L-Phg-OH are dissolved in 300 ml of dry tetrahydrofuran, and 13.55 ml (97 mmoles) of triethylamine are added to the solution. The mixture is cooled to -10° C., and 12.1 ml (97 mmoles) of pivaloyl chloride are introduced. The suspension of the mixed anhydride is stirred for 10 minutes at -10° C., thereafter cooling is stopped and ammonia is bubbled through the suspension for one hour. Next day the reaction mixture is evaporated, and the residue is processed as described for the D enantiomer. 18.90 g (68.7%) of Z-L-Phg-NH2 are obtained; m.p.: 172°-173° C., Rf4 =0.75, [α]D =+80.7° (c=1.0, in dimethyl formamide).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04183909 |
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| 出典データセット | uspto-grants-1980_01 |
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| ORD ID | ord-a6ab6b5dde2c43febb1212f6add3fe4a |
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| 出典メモ | uspto-grants-1980_01 |
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