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HRID 1010543作成日:2026年10月27日
Sulfuric acid magnesium salt (1:1) → (tert-butoxy)-N-(2-{[(2-chloro(1,3-thiazol-5-yl))methyl][(4-methoxyphenyl)methyl]amino}ethyl)carboxamide
https://huagongshe.com/reaction/1010543
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 | 2-Chloro-1,3-thiazole-5-carbaldehyde | HCID 1479765 | — |
| 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-{[(2-chloro(1,3-thiazol-5-yl))methyl][(4-methoxyphenyl)methyl]amino}ethyl)carboxamide | HCID 131728996 | 68.5% |
反応手順
This compound was also made in a manner analogous to that set forth in Step D of Example 5, and Step A above, using 0.25 gram (0.0017 mole) of (2-chloro-1,3-thiazol-5-yl)formaldehyde, 0.47 gram (0.0017 mole) of (tert-butoxy)-N-(2-{[(4-methoxyphenyl)methyl]amino}ethyl)carboxamide, 0.54 gram (0.0025 mole) of sodium triacetoxyborohydride and 0.40 gram (0.0034 mole) of magnesium sulfate in about 10 mL of 1,2-dichloroethane. The reaction product was purified with column chromatography on silica gel. In a first chromatography, elution was accomplished using mixtures of 2% to 5% methanol in methylene chloride as eluants. In a second chromatography, elution was accomplished using a mixture of 1.5% methanol in methylene chloride as an eluant. Appropriate fractions were combined and concentrated under reduced pressure, yielding 0.48 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-08bb04552a9841a980feb4305c89d2e8 |
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| 出典メモ | uspto-grants-2011_07 |
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