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Tributyltin azide → N-Ethyl-N'-[6-(2H-1,2,3,4-tetraazol-5-yl)-1,3-benzothiazol-2-yl]urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributyltin azide | HCID 4984872 | — |
| 反応物 | N-(6-Cyano-1,3-benzothiazol-2-yl)-N'-ethylurea | HCID 21985533 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-Ethyl-N'-[6-(2H-1,2,3,4-tetraazol-5-yl)-1,3-benzothiazol-2-yl]urea | HCID 21985643 | — |
反応手順
About 30 mg N-(6-cyano-1,3-benzothiazol-2-yl)-N′-ethylurea was charged into about 5 mL dry tetrahydrofuran. Added about 2 g of azidotributylstannane then refluxed for about 48–72 hours. The solvent was removed under reduced pressure then the crude oil was taken up in dichloromethane. About 0.5 mL of dilute aqueous hydrochloric acid was added and a white precipitate formed. This was allowed to sit for about 30 minutes then the precipitate was collected by filtration, washed with warm THF then dried under vacuum. 1H NMR 1.10 (t, 3H), 3.2 (m, 2H), 6.76 (br s, 1H), 7.78 (d, 1H), 8.0 (d, 1H), 8.58 (s, 1H), 10.91 (s, 1H); LC/MS 1.37 min, 290 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091227B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-1c22368b0e704f58812f062c12896e4b |
| 出典メモ | uspto-grants-2006_08 |