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Tetrahydrothiopyran-4-one → 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro-[2H-1,3-benzoxazine-2,4'-tetrahydrothiopyran]
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrothiopyran-4-one | HCID 66173 | — |
| 反応物 | 2-Aminomethyl-4-t-butyl-6-iodophenol | HCID 119286 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro-[2H-1,3-benzoxazine-2,4'-tetrahydrothiopyran] | HCID 12857899 | 62% |
反応手順
A mixture of 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol (3.0 g., 0.01 mole), tetrahydrothiopyran-4-one (1.18 g., 0.01 mole), and benzene (100 ml.), is refluxed under a Dean-Stark trap for 4 hr. The solvent is evaporated, and the residue is crystallized from ethanol to obtain 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro-[2H-1,3-benzoxazine-2,4'-tetrahydrothiopyran], (2.5 g.), m.p. 123°-124° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04092414 |
| 出典データセット | uspto-grants-1978_05 |
| ORD ID | ord-3ecb22d8e9f54b36971f396c14b4a2c7 |
| 出典メモ | uspto-grants-1978_05 |