関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | 4-Methoxybenzaldehyde | HCID 31244 | — |
| 反応物 | N-BOC-ethylenediamine | HCID 187201 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | Tert-butyl N-(2-{[(4-methoxyphenyl)methyl]amino}ethyl)carbamate | HCID 112688707 | 11.7% |
反応手順
This compound was made in a manner analogous to that set forth in Step D of Example 5, using 3.0 grams (0.022 mole) of 4-methoxybenzaldehyde, 3.6 grams (0.022 mole) of N-(2-aminoethyl)(tert-butoxy)carboxamide (known compound), 7.0 grams (0.033 mole) of sodium triacetoxyborohydride and 5.3 grams (0.044 mole) of magnesium sulfate in 30 mL of 1,2-dichloroethane. The reaction product was purified with column chromatography on silica gel. Elution was accomplished using mixtures of 2% to 5% methanol in methylene chloride as eluants. Appropriate fractions were combined and concentrated under reduced pressure, yielding 0.72 gram of the subject compound. The NMR spectrum was consistent with the proposed structure. The reaction was repeated to obtain additional material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07977332B2 |
|---|
| 出典データセット | uspto-grants-2011_07 |
|---|
| ORD ID | ord-2837d5fa729442a4be30e1e0928e643f |
|---|
| 出典メモ | uspto-grants-2011_07 |
|---|