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Tris(hydroxymethyl)aminomethane → Methyl {4-[({[(4-tert-butylphenyl)amino]carbonyl}{4-[(4-butylphenyl)-ethynyl]benzyl}amino)methyl]phenoxy}acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 1-Tert-butyl-4-isocyanatobenzene | HCID 2735695 | — |
| 反応物 | Methyl {4-[({4-[(4-butylphenyl)ethynyl]benzyl}amino)methyl]phenoxy}acetate | HCID 57554567 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl {4-[({[(4-tert-butylphenyl)amino]carbonyl}{4-[(4-butylphenyl)-ethynyl]benzyl}amino)methyl]phenoxy}acetate | HCID 11541808 | — |
反応手順
A solution of methyl {4-[({4-[(4-butylphenyl)ethynyl]benzyl}amino)methyl]phenoxy}acetate (45 mg, 0.10 mmol) and 4-tert-butylphenylisocyanate (Aldrich, 27 mg, 0.15 mmol) in DCM (2 mL) was stirred at rt overnight in presence of a morpholine resin (1.5 eq., Novabiochem HL, 3.8 mmol/g). Trisamine resin (1.2 eq, Novabiochem, 3.5 mmol/g) was then added and the mixture was stirred at rt for an additional 2 hrs. The reaction mixture was then filtrated and the solvent was removed under reduced pressure to give quantitatively the title compound. HPLC, Rt: 5.97 min purity: 96.3%). M+(ESI): 619.6, M−(ESI): 616.9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07947851B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-e3844b273548408292ebf116bfd0dabc |
| 出典メモ | uspto-grants-2011_05 |