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HRID 14411作成日:2026年10月26日

Benzaldehyde → 9-Amino-19-benzyl-14,32-dichloro-5-methyl-26-oxa-4-thia-3,8,10,16,19-pentaazatetracyclo[25.2.2.212,15.02,6] tritriaconta-1(29),2,5,8,12,14,23,27,30,32-decaene-7,17-dione

https://huagongshe.com/reaction/14411

反応式

関与物質

役割名称HCID仕込み量
反応物BenzaldehydeHCID 240—
反応物Trimethyl orthoformateHCID 9005—
反応物Sodium triacetoxyborohydrideHCID 5049666—
反応物9-Amino-14,32-dichloro-5-methyl-26-oxa-4-thia-3,8,10,16,19-pentaazatetracyclo[25.2.2.212,15.02,6]tritriaconta-1(29),2,5,8,12,14,23,27,30,32-decaene-7,17-dioneHCID 178435148—
溶媒Acetic AcidHCID 176—
生成物9-Amino-19-benzyl-14,32-dichloro-5-methyl-26-oxa-4-thia-3,8,10,16,19-pentaazatetracyclo[25.2.2.212,15.02,6] tritriaconta-1(29),2,5,8,12,14,23,27,30,32-decaene-7,17-dioneHCID 178435147—

反応手順

The cis/trans mixture of the title compound of 9-amino-14,32-dichloro-5-methyl-26-oxa-4-thia-3,8,10,16,19-pentaazatetracyclo[25.2.2.212,15.02,6]tritriaconta-1(29),2,5,8,12,14,23,27,30,32-decaene-7,17-dione (Example 4) (60 mg), benzaldehyde (24 mg), sodium triacetoxyborohydride (30 mg), trimethyl orthoformate (0.2 mL) and acetic acid (0.1 mL), in 2 mL of DMF was stirred at room temperature for 16 hrs. Ethyl acetate (10 mL) and saturated sodium bicarbonate solution (10 mL) were added. Layers were separated after the mixture was well shaken. The organic layer was dried over anhydrous magnesium sulfate and solvent was evaporated in vacuo to give a crude product, which was purified by preparative HPLC to give 27 mg of the title compound as an inseparable mixture of cis/trans isomers.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07732434B2
出典データセットuspto-grants-2010_06
ORD IDord-8585272f986b43429b57b80fb10e19a7
出典メモuspto-grants-2010_06