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3,4-dihydro-2H-pyran → 2-[(6-bromohexyl)oxy]tetrahydro-2H-pyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 反応物 | 6-Bromo-1-hexanol | HCID 77970 | — |
| 生成物 | 2-[(6-bromohexyl)oxy]tetrahydro-2H-pyran | HCID 103860 | 91.1% |
反応手順
6-bromo-1-(tetrahydropyranyloxy)hexane was synthesized in the same manner as in Example 1 (the formula (26): step 1). First, 197.8 g (1.09 mol) of 6-bromo-1-hexanol were fed into a 500 mL reactor vessel and cooled to 5° C. or less, and then 102.1 g (1.21 mol) of dihydropyran were dripped at 10° C. or less. After completion of dripping, the mixture was warmed to room temperature and stirred for one hour. The obtained residues were subjected to silica gel column and purified using a mixed solvent of hexane/diisopropylether (IPE) (volume ratio 5:1) as an eluting solvent, and thus 263.4 g of 6-bromo-1-(tetrahydropyranyloxy)hexane were obtained. The yield in this case was 90.9%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560731B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-b00c6b0673e34209909a03f73c6ad8ac |
| 出典メモ | uspto-grants-2009_07 |