関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | (2S)-3,4-dihydro-2H-1-benzopyran-2-carboxylic acid | HCID 6933105 | — |
| 生成物 | Isobutyl (S)-chroman-2-carboxylate | HCID 54151958 | — |
反応手順
The aqueous phase of the hydrolysis reaction was acidified to pH of 2.0 with conc. HCl forming a white precipitate of (S)-chroman-2-carboxylic acid. The S-acid was extracted into toluene, and the phases were separated. The organic layer was placed in a vessel suitable for acid catalyzed esterification. Sulfuric acid was added to the vessel, and the mixture was heated to reflux. Water was removed by azeotropic distillation. The conversion of the acid to the ester was followed by GC analysis. Isobutyl (S)-chroman-2-carboxylate was thereby formed. Upon completion of the esterification, the sulfuric acid catalyst used in the reaction was removed by washing the reaction product with saturated sodium carbonate, and the S-carboxylate product was azeotropically dried again.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05658796 |
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| 出典データセット | uspto-grants-1997_08 |
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| ORD ID | ord-509626b07857430d8702245ebee2df6d |
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| 出典メモ | uspto-grants-1997_08 |
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