反応 #4027417
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2cc16d2b875b4d56ab051a691f24297f表示可能な構造データがありません
C1=C(C=C(C=C1O)O)C(=O)N製品情報
3,5-dihydroxybenzamide (CAS 3147-62-4) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 76604
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
6 反応 · 6 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2cc16d2b875b4d56ab051a691f24297f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: After reaction step (a), the resulting amine (1 equiv.), 3,5-dihydroxybenzoic acid (1 equiv.), EDCI (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) (1.2 equiv.), HOBt (1-hydroxybenzotriazole hydrate) (1.2 equiv.), and Et3N (4 equiv.) in CH2Cl2.DMF (9:1) were stirred for 12 hours at room temperature. Then the reaction mixture was diluted with EtOAc and the organic layer washed with brine. The combined organic layer was dried over anhydrous Na2SO4 and concentrated. Purification of the resulting crude product by flash silica gel chromatography provided corresponding 3,5-dihydroxybenzamide derivative. The above derivative (1 equiv.) and active carbonate 4 (1.1 equiv.) in THF were stirred under hydrogen atmosphere in presence of Pd—C (10%) for 12 hours at room temperature. Then the reaction mixture was filtered and the organic layer washed with brine. The combined organic layer was dried over anhydrous Na2SO4 and concentrated. Purification of the resulting crude product by flash silica gel chromatography provided compound 134 as a solid. After reaction step (a) the organic layer washed with brine The combined organic layer was dried over anhydrous Na2SO4 concentrated Purification of the resulting crude product by flash silica gel chromatography
ソース ID: ord-7efcf994c2e943c1970d84ab2f92882f反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2cc16d2b875b4d56ab051a691f24297f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: After reaction step (a), the resulting amine (1 equiv.), 3,5-dihydroxybenzoic acid (1 equiv.), EDCI (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) (1.2 equiv.), HOBt (1-hydroxybenzotriazole hydrate) (1.2 equiv.), and Et3N (4 equiv.) in CH2Cl2.DMF (9:1) were stirred for 12 hours at room temperature. Then the reaction mixture was diluted with EtOAc and the organic layer washed with brine. The combined organic layer was dried over anhydrous Na2SO4 and concentrated. Purification of the resulting crude product by flash silica gel chromatography provided corresponding 3,5-dihydroxybenzamide derivative. The above derivative (1 equiv.) and active carbonate 4 (1.1 equiv.) in THF were stirred under hydrogen atmosphere in presence of Pd—C (10%) for 12 hours at room temperature. Then the reaction mixture was filtered and the organic layer washed with brine. The combined organic layer was dried over anhydrous Na2SO4 and concentrated. Purification of the resulting crude product by flash silica gel chromatography provided compound 134 as a solid. After reaction step (a) the organic layer washed with brine The combined organic layer was dried over anhydrous Na2SO4 concentrated Purification of the resulting crude product by flash silica gel chromatography
ソース ID: ord-c781951f050045288ea58b6dbd9a58ca反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: After reaction step (a), the resulting amine (1 equiv.), 3,5-dihydroxybenzoic acid (1 equiv.), EDCI (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) (1.2 equiv.), HOBt (1-hydroxybenzotriazole hydrate) (1.2 equiv.), and Et3N (4 equiv.) in CH2Cl2.DMF (9:1) were stirred for 12 hours at room temperature. Then the reaction mixture was diluted with EtOAc and the organic layer washed with brine. The combined organic layer was dried over anhydrous Na2SO4 and concentrated. Purification of the resulting crude product by flash silica gel chromatography provided corresponding 3,5-dihydroxybenzamide derivative. The above derivative (1 equiv.) and active carbonate 4 (1.1 equiv.) in THF were stirred under hydrogen atmosphere in presence of Pd—C (10%) for 12 hours at room temperature. Then the reaction mixture was filtered and the organic layer washed with brine. The combined organic layer was dried over anhydrous Na2SO4 and concentrated. Purification of the resulting crude product by flash silica gel chromatography provided compound 134 as a solid. After reaction step (a) the organic layer washed with brine The combined organic layer was dried over anhydrous Na2SO4 concentrated Purification of the resulting crude product by flash silica gel chromatography
ソース ID: ord-7efcf994c2e943c1970d84ab2f92882f反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2cc16d2b875b4d56ab051a691f24297fPubChem References
化合物の公開データベース記録に掲載された情報源です。
