関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | Boron trifluoride | HCID 6356 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 7-Aminocephalosporanic acid | HCID 441328 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 3-Benzyloxy-7-amino-ceph-3-eme-4-carboxylic acid | HCID 131718115 | — |
反応手順
Using the procedure of Step A of Example 8, 27.2 g of 7-amino-cephalosporanic acid, 128 ml of the etherate of boron trifluoride, 126 ml of benzyl alcohol and 90 ml of triethylamine were reacted to obtain 27.1 g of raw product. 25 g of the said product and 250 ml of acetic acid were added to 25 ml of the etherate of boron trifluoride followed by the addition of 25 ml of triethylamine which caused precipitation. The mixture was vacuum filtered and the product was rinsed with acetic acid, acetone and then ether to obtain 4.6 of product. 4.8 g of the said product were dissolved at 45° C. in 20 ml of 2N hydrochloric acid and 8 ml of concentrated hydrochloric acid and the solution was treated with activated carbon. 6 ml of ammonium hydroxide were added to the mixture which was then vacuum filtered. The product was rinsed with water, acetone and then ether to obtain 2 g of 3-benzyloxy-7-amino-ceph-3-eme-4-carboxylic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05243043 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-80f62c1c46ba4eb9a6ba6a91577ca2ab |
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| 出典メモ | uspto-grants-1993_09 |
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