関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | N-trityl piperazine, succinate salt | HCID 67005131 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Trityl piperazine phenyl carbamate | HCID 86622265 | 80% |
反応手順
To a cooled suspension of compound 11 in dichloromethane (6 mL/g 11) was added a solution of potassium carbonate (3.2 eq) in water (4 mL/g potassium carbonate). To this two-phase mixture was slowly added a solution of phenyl chloroformate (1.03 eq) in dichloromethane (2 g/g phenyl chloroformate). The reaction mixture was warmed to 20° C. Upon reaction completion (1-2 hr), the layers were separated. The organic layer was washed with water, and dried over anhydrous potassium carbonate. The product 35 was isolated by crystallization from acetonitrile. Yield=80%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07943762B2 |
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| 出典データセット | uspto-grants-2011_05 |
|---|
| ORD ID | ord-7e6befc7fb464f178d201e76a0cb307e |
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| 出典メモ | uspto-grants-2011_05 |
|---|
