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Cyclohexanone → 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro[2H-1,3-benzoxazine-2,1'-cyclohexane]
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyclohexanone | HCID 7967 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | 2-Aminomethyl-4-t-butyl-6-iodophenol | HCID 119286 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro[2H-1,3-benzoxazine-2,1'-cyclohexane] | HCID 12857892 | 72.7% |
反応手順
A mixture of 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol (1.5 g., 0.005 mole), cyclohexanone (0.5 g., 0.005 mole), and magnesium sulfate (0.5 g.) in tetrahydrofurane (50 ml.) is kept under nitrogen at 20°-25° C., for 16 hours. The magnesium sulfate is removed and the filtrate evaporated to dryness. The residue is crystallized from ethanol to obtain 3,4-dihydro-6-(1,1-dimethylethyl)-8-iodospiro[2H-1,3-benzoxazine-2,1'-cyclohexane] (1.4 g.), m.p. 112°-114° 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-5aea0e76281a433ea39b979896e6e638 |
| 出典メモ | uspto-grants-1978_05 |