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3-(Methylthio)-1-propanol → (3-(3-Bromo-2-methylphenoxy)propyl)(methyl)sulfane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-(Methylthio)-1-propanol | HCID 10448 | — |
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 反応物 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 反応物 | 3-Bromo-2-methylphenol | HCID 11171430 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (3-(3-Bromo-2-methylphenoxy)propyl)(methyl)sulfane | HCID 86697160 | — |
反応手順
3-Bromo-2-methylphenol (0.10 g), 3-(methylthio)propanol (0.055 mL), tri-n-butyl phosphine (0.12 g) and 1,1′-(azodicarbonyl)dipiperidine (0.15 g) are stirred in tetrahydrofurane for 16 hours. Water is added and the mixture extracted with diethyl ether. The organic layer is washed with brine, dried (Na2SO4) and volatiles removed under reduced pressure. The product (80 mg) is obtained after column chromatography (silica gel, n-hexane/ethyl acetate gradient 100:0 to 50:50).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08642585B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-ef70e29ed21546b2a8527d437f2c62ee |
| 出典メモ | uspto-grants-2014_02 |