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HRID 1010545作成日:2026年10月27日
Sulfuric acid magnesium salt (1:1) → (tert-butoxy)-N-(2-{[(4-methoxyphenyl)methyl](oxolan-3-ylmethyl)amino}ethyl)carboxamide
https://huagongshe.com/reaction/1010545
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 | 3-Furancarboxaldehyde, tetrahydro- | HCID 157568 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | Tert-butyl N-(2-{[(4-methoxyphenyl)methyl]amino}ethyl)carbamate | HCID 112688707 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | (tert-butoxy)-N-(2-{[(4-methoxyphenyl)methyl](oxolan-3-ylmethyl)amino}ethyl)carboxamide | HCID 131728997 | 80.9% |
反応手順
This compound was made in a manner analogous to that set forth in Step D of Example 5, using 0.2 gram (0.0020 mole) of (oxolan-3-yl)formaldehyde, 0.56 gram (0.0020 mole) of (tert-butoxy)-N-(2-{[(4-methoxyphenyl)methyl]amino}-ethyl)carboxamide (prepared in Step A of Example 9), 0.64 gram (0.0030 mole) of sodium triacetoxyborohydride and 2.5 grams (0.021 mole) of magnesium sulfate in 50 mL of 1,2-dichloroethane. The reaction product was purified with column chromatography on silica gel. Elution was accomplished using a mixture of 1% methanol in methylene chloride as an eluant. Appropriate fractions were combined and concentrated under reduced pressure, yielding 0.59 gram of the subject compound. The NMR spectrum was consistent with the proposed structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07977332B2 |
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| 出典データセット | uspto-grants-2011_07 |
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| ORD ID | ord-ab9d4328df8b41dcbeb9a02578764ec8 |
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| 出典メモ | uspto-grants-2011_07 |
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