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HRID 735829作成日:2026年10月26日

1,2-Dichloroethane → HCID 178443268、化合物

https://huagongshe.com/reaction/735829

反応式

関与物質

役割名称HCID仕込み量
反応物1,2-DichloroethaneHCID 11—
反応物4-({(tert-butoxycarbonyl)[4-(trifluoromethyl)benzyl]amino}methyl)-benzoic AcidHCID 67188599—
反応物N'-hydroxydodecanimidamideHCID 178443266—
触媒4-(Dimethylamino)pyridineHCID 14284—
溶媒DichloromethaneHCID 6344—
生成物HCID 178443268HCID 17844326824%

反応手順

To a solution of 4-({(tert-butoxycarbonyl)[4-(trifluoromethyl)benzyl]amino}methyl)-benzoic acid (102 mg, 0.25 mmol), N-hydroxydodecanimidamide (70 mg, 0.33 mmol) and DMAP (3 mg, 0.03 mmol) in anhydrous DCM (15 mL) was added EDC (62 mg, 0.33 mmol) and the resulting reaction mixture was stirred at RT for 14 h. Evaporation of the solvents gave an oil. This crude product was purified by column chromatography over silica gel (AcOEt/c-Hex 80/20) to give the title compound as a colorless oil (36 mg, 24%). 1H NMR (CDCl3, 300 MHz) δ 8.01 (d, J=8.1 Hz, 2H), 7.60 (d, J=8.1 Hz, 2H), 7.40-7.20 (m, 4H), 4.88 (br s, 2H), 4.51 (s, 2H), 4.42 (s, 2H), 2.36 (t, J=8.2 Hz, 2H), 1.75-1.59 (m, 2H), 1.49 (s, 9H), 1.45-1.16 (m, 16H), 0.89 (t, J=7.0 Hz, 3H). HPLC (Condition A), Rt: 5.42 min (HPLC purity: 96.1%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07592477B2
出典データセットuspto-grants-2009_09
ORD IDord-3d861b7ed7a5412fa1471881905def9b
出典メモuspto-grants-2009_09