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Trichloroacetic Acid → ASTA-Z-7654(free acid)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trichloroacetic Acid | HCID 6421 | — |
| 反応物 | 4-Hydroxycyclophosphamide | HCID 99735 | — |
| 反応物 | 2-Sulfanylethane-1-sulfonic acid--cyclohexanamine (1/1) | HCID 23049873 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | ASTA-Z-7654(free acid) | HCID 6917796 | — |
反応手順
1.4 g (5 mmol) of 4-hydroxycyclophosphamide and 1.2 g (5 mmol) of cyclohexylammonium-2-mercaptoethanesulphonate were dissolved together with a trace of trichloroacetic acid in 25 ml of methanol and were left to stand overnight in a refrigerator at -25° C. The reaction solution was then concentrated to about 5 ml, ether was added until clouding commenced and the mixture was triturated. The crystallised material was filtered with suction after standing for 20 hours at 0° C., and was washed and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04623742 |
| 出典データセット | uspto-grants-1986_11 |
| ORD ID | ord-78d36a09114c45999debc021d0f1fa0b |
| 出典メモ | uspto-grants-1986_11 |