関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylcarbodiimide | HCID 12734 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 反応物 | 4-Methyl-4-(methyldisulfanyl)pentanoic acid | HCID 11564634 | — |
| 反応物 | HCID 57570932 | HCID 57570932 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 57570917 | HCID 57570917 | 54.7% |
反応手順
To a solution of 1-(3-amino-propyloxy)-3,5-bis-(hydroxymethyl)-benzene (50 mg) in dimethylformamide (1 mL) was added 4-methyl-4-methyldisulfanyl-pentanoic acid (44 mg), N,N′-diisopropylcarbodiimide (35 mL) and 1-hydroxybenzotriazole hydrate (5.8 mg). After 15 h at room temperature, water was added to the reaction mixture and the aqueous solution was extracted twice with ethyl acetate. The combined organic solutions were washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate and concentrated in vacuo to a residue. The residue was purified by silica gel chromatography (Interchrom Puriflash 5 g column, SiOH 15-35 μm), eluted with methanol/dichloromethane, 5:95 to give 1-[3-(4-methyl-4-methyldisulfanyl-pentanoylamino)-propyloxy]-3,5-bis-(hydroxymethyl)-benzene (48 mg):
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08163736B2 |
|---|
| 出典データセット | uspto-grants-2012_04 |
|---|
| ORD ID | ord-4fd01d9b94d3461a923c3c3589789e1e |
|---|
| 出典メモ | uspto-grants-2012_04 |
|---|