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Hydrochloric Acid → benzyl N-[4-(azidomethyl)benzenecarboximidoyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | 4-Amidino benzyl azide | HCID 22257605 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | benzyl N-[4-(azidomethyl)benzenecarboximidoyl]carbamate | HCID 140379073 | — |
反応手順
The crystals from (ii) above were dissolved in 500 ml methylene chloride and the resulting solution was dried (K2CO3), filtered and 27 ml (194 mmol) triethyl amine was added. 25 ml Benzyl chloroformate was slowly added to the stirred solution while the reaction mixture was cooled in an ice bath. After 30 minutes an additional 2 ml benzyl chloroformate was added and stirring was continued for another 30 minutes. Subsequently water was added and the aqueous phase was adjusted to pH 7 with 2M HCl. The organic phase was dries (MgSO4) and the solvent was removed in vacuo. 4-(benzyloxycarbonylamidino) benzyl azide was finally isolated as colorless crystals from ether/methylene chloride/hexane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05780631 |
| 出典データセット | uspto-grants-1998_07 |
| ORD ID | ord-5a8cc25184054f9e9f979b9a2d2552b5 |
| 出典メモ | uspto-grants-1998_07 |