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HRID 1049867作成日：2026年10月27日
Diisopropylethylamine → 3-[5-(2-Acetoxy-2-methyl-propionylamino)-4-carbamoyl-thiophen-2-ylsulfanyl]-propionic acid 2-ethyl-hexyl ester
https://huagongshe.com/reaction/1049867
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Ethylhexyl 3-mercaptopropionate | HCID 92640 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | [2-[(5-Bromo-3-carbamoyl-2-thienyl)amino]-1,1-dimethyl-2-oxo-ethyl]acetate | HCID 117717729 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-[5-(2-Acetoxy-2-methyl-propionylamino)-4-carbamoyl-thiophen-2-ylsulfanyl]-propionic acid 2-ethyl-hexyl ester | HCID 117717785 | — |
反応手順
Intermediate 11 (1.4 g, 4 mmol) is dissolved in toluene (16 mL) and DIEA (1.4 mL, 8 mmol). Next, Pd2dba3 (110 mg, 0.12 mmol), Xantphos (139 mg, 0.24 mmol) and 3-Mercaptopropionic acid 2-ethylhexylester (1.14 mL, 5 mmol) are added, and the resulting solution is flushed with N2. Reaction mixture is stirred at 110° C. overnight. After evaporation, the crude is purified using column chromatography. The resulting product is obtained as an oil, which crystallised overnight. Obtained product is used as such.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09382254B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-c686567f3d01469b809b2228195b9e7b |
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| 出典メモ | uspto-grants-2016_07 |
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