4-Methoxybenzylamine → N-(4-methoxybenzyl)-2-(4-chlorophenyl hydrazono) propionic acid amide

HRID 859849

반응식

HRID 859849 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][N:9]=[C:10]([CH3:14])[C:11]([OH:13])=O)=[CH:4][CH:3]=1.C(C1NC=CN=1)(C1NC=CN=1)=O.[CH3:27][O:28][C:29]1[CH:36]=[CH:35][C:32]([CH2:33][NH2:34])=[CH:31][CH:30]=1>O1CCCC1>[CH3:27][O:28][C:29]1[CH:36]=[CH:35][C:32]([CH2:33][NH:34][C:11](=[O:13])[C:10](=[N:9][NH:8][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[CH3:14])=[CH:31][CH:30]=1

참가 물질

5

반응물 3

HCID 754524-MethoxybenzylamineHCID 2284632-[2-(4-Chlorophenyl)hydrazinylidene]propanoic acidHCID 5250894Bis-(1H-imidazol-2-YL)-methanone

생성물 1

HCID 86600613N-(4-methoxybenzyl)-2-(4-chlorophenyl hydrazono) propionic acid amide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

2-(4-Chlorophenyl hydrazono) propionic acid (0.64 g, 3.0 mmol) was dissolved in tetrahydrofuran (3 ml), and carbonyl diimidazole (0.49 g, 3.0 mmol) was added under cooling with ice. After stirring at room temperature for 1 hour, a solution of 4-methoxybenzyl amine (0.41 g, 3.0 mmol) in tetrahydrofuran (3 ml) was added thereto. 15 hours later, the mixture was washed with 6N hydrocloric acid, 1N aqueous solution of sodium hydroxide and a saturated brine, dried on sodium sulfate and then filtered. The residue obtained by concentrating the resulting filtrate was suspended in a mixed solvent of hexane and chloroform (1:1) and filtered to obtain N-(4-methoxybenzyl)-2-(4-chlorophenyl hydrazono) propionic acid amide (Compound No. 93) (0.76 g, 2.3 mmol, 76%).

후처리

  1. temperatureunder cooling with ice
  2. wash15 hours later, the mixture was washed with 6N hydrocloric acid, 1N aqueous solution of sodium hydroxide
  3. dry with materiala saturated brine, dried on sodium sulfate
  4. filtrationfiltered
  5. customThe residue obtained
  6. concentrationby concentrating the resulting filtrate
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-59d318124f7c4099b877d80a74366255
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07153815B2

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