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Triethylamine → 4-[[(N-(2-(tert-butoxycarbonylamino)-4,5-difluorobenzoyl)glycyl)amino]methyl]-1-(4-chlorobenzyl)piperidine

HRID 279321
ノート
印刷プレビュー

反応式

HRID 279321 の反応式
Cl.Cl.[Cl:3][C:4]1[CH:22]=[CH:21][C:7]([CH2:8][N:9]2[CH2:14][CH2:13][CH:12]([CH2:15][NH:16][C:17](=[O:20])[CH2:18][NH2:19])[CH2:11][CH2:10]2)=[CH:6][CH:5]=1.CCN(CC)CC.[C:30]([O:34][C:35]([NH:37][C:38]1[CH:46]=[C:45]([F:47])[C:44]([F:48])=[CH:43][C:39]=1[C:40](O)=[O:41])=[O:36])([CH3:33])([CH3:32])[CH3:31].CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>[OH-].[Na+]>[C:30]([O:34][C:35]([NH:37][C:38]1[CH:46]=[C:45]([F:47])[C:44]([F:48])=[CH:43][C:39]=1[C:40]([NH:19][CH2:18][C:17]([NH:16][CH2:15][CH:12]1[CH2:11][CH2:10][N:9]([CH2:8][C:7]2[CH:21]=[CH:22][C:4]([Cl:3])=[CH:5][CH:6]=2)[CH2:14][CH2:13]1)=[O:20])=[O:41])=[O:36])([CH3:33])([CH3:31])[CH3:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 184261442-((Tert-butoxycarbonyl)amino)-4,5-difluorobenzoic acidHCID 184261541-(4-Chlorobenzyl)-4-[(glycylamino)methyl]piperidine dihydrochloride

生成物 1

HCID 18426199
4-[[(N-(2-(tert-butoxycarbonylamino)-4,5-difluorobenzoyl)glycyl)amino]methyl]-1-(4-chlorobenzyl)piperidine
収率 92%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 1-(4-chlorobenzyl)-4-{(glycylamino)methyl}piperidine dihydrochloride (738 mg, 2 mmol) in CH2Cl (20 mL) was treated with Et3N (1.1 mL, 8 mmol), 2-(tert-butoxycarbonylamino)-4,5-difluorobenzoic acid (607 mg, 2.2 mmol), EDCI (422 mg, 2.2 mmol) and HOBt (337 mg, 2.2 mmol). After the reaction mixture was stirred at room temperature for 14 h, 0.6 N aqueous NaOH solution (50 mL) was added, and the mixture was extracted with dichloromethane (3 times). The combined organic layers were dried over anhydrous sodium sulfate, filtered, and concentrated. Column chromatography (SiO2, ethyl acetate then ethyl acetate/methanol=92/8) afforded the desired 4-[{(N-(2-(tert-butoxycarbonylamino)-4,5-difluorobenzoyl)glycyl)amino}methyl]-1-(4-chlorobenzyl)piperidine (1.01 g, 92%): ESI/MS m/e 551.3 (M++H, C27H33ClF2N4O4).

後処理

  1. extractionthe mixture was extracted with dichloromethane (3 times)
  2. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-639af57812b7463084b6cec63b5e5d8d
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06362177B1

反応ノート

読み込み中…

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