関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 2-Amino-6-thiocyanato-1,3-benzothiazole | HCID 81600 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Phenyl(6-thiocyanato-1,3-benzothiazol-2-yl)carbamate | HCID 53472570 | 87.4% |
反応手順
7.5 g of phenyl chlorocarbonate and then 4.05 g of sodium hydrogen carbonate and 9.4 cm3 of water are added, at 20° C., to a solution of 2.5 g of commercial 2-amino-1,3-benzothiazol-6-yl thiocyanate in 94 cm3 of tetrahydrofuran. The resulting mixture is subsequently stirred at 20° C. for 20 h and then extracted with 2×150 cm3 of ethyl acetate. The organic phases are combined and then washed with 3×50 cm3 of a saturated aqueous solution of sodium hydrogen carbonate. The organic phase obtained is dried over magnesium sulphate and then concentrated to dryness under reduced pressure. The residue is taken up in 50 cm3 of water and the product is spin-filter-dried and dried under vacuum at 20° C. 3.45 g of phenyl (6-thiocyanato-1,3-benzothiazol-2-yl)carbamate are thus obtained in the form of a pale yellow solid, the characteristics of which are as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09321777B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-c272f38368304f7a8bae2b6dc16aab76 |
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| 出典メモ | uspto-grants-2016_04 |
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