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HRID 355929作成日:2026年10月26日

2-Methylbenzyl alcohol → (2-Methylphenyl)methyl 4-[(6,11-dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl)benzoate

https://huagongshe.com/reaction/355929

反応式

関与物質

役割名称HCID仕込み量
反応物2-Methylbenzyl alcoholHCID 6994—
反応物Sodium hydrideHCID 24758—
反応物4-[(6,11-dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl]benzoyl chlorideHCID 53802244—
溶媒TetrahydrofuranHCID 8028—
生成物(2-Methylphenyl)methyl 4-[(6,11-dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl)benzoateHCID 8675157532%

反応手順

To a mixture of 248 mg of 2-methylbenzyl alcohol in 4 ml of anhydrous tetrahydrofuran is added 80 mg of sodium hydride (60% in mineral oil) and the mixture stirred for 1 hour. To the mixture is added 430 mg of 4-[(6,11-dihydro-5H-dibenz[b,e]azepin-5-yl)-carbonyl]benzoyl chloride and the mixture is stirred for 18 hours. The tetrahydrofuran is evaporated in vacuo to a residue which is partitioned between methylene chloride and water. The organic layer is separated and washed with 1N HCl, water, 1M NaHCO3, and brine. The organic layer is dried (Na2SO4) and passed through a short pad of hydrous magnesium silicate and hexane added at the boil to give 170 mg of the desired product, m.p. 140°-142° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05834461
出典データセットuspto-grants-1998_11
ORD IDord-03aee920d8d24760bae861837452bc89
出典メモuspto-grants-1998_11