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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 70095412、化合物

HRID 868914
ノート
印刷プレビュー

反応式

HRID 868914 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]=[CH:3][C:2]=1[CH2:11][CH2:12][C:13]([OH:15])=[O:14].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.[N:37]1[C:46]2[C:41](=[C:42]([NH2:48])[C:43]([NH2:47])=[CH:44][CH:45]=2)[CH:40]=[CH:39][CH:38]=1>C(Cl)Cl>[NH2:48][C:42]1[C:43]([NH:47][C:13](=[O:15])[CH2:12][CH2:11][C:2]2[CH:3]=[N:4][C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[N:1]=2)=[CH:44][CH:45]=[C:46]2[C:41]=1[CH:40]=[CH:39][CH:38]=[N:37]2.[NH2:47][C:43]1[C:42]([NH:48][C:13](=[O:14])[CH2:12][CH2:11][C:2]2[CH:3]=[N:4][C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[N:1]=2)=[C:41]2[C:46](=[CH:45][CH:44]=1)[N:37]=[CH:38][CH:39]=[CH:40]2
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 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 2925043-(Quinoxalin-2-yl)propanoic acidHCID 426874Quinoline-5,6-diamine

生成物 2

HCID 70095412HCID 70095412、化合物HCID 70097400HCID 70097400、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-(quinoxalin-2-yl)propanoic acid (550 mg, 2.7 mmol) in DCM (30 mL) was added HOBt (550 mg, 4 mmol) and EDCI (780 mg, 4 mmol). After stirring for 30 minutes, quinoline-5,6-diamine (430 mg, 2.7 mmol) was added and the reaction was stirred for 3 hours. The mixture was washed with water (10 mL) and extracted with DCM (30 mL×3). The combined organic layers were dried over sodium sulfate, filtered, and concentrated to afford a yellow mixture which was purified by reverse phase chromatography. N-(5-Aminoquinolin-6-yl)-3-(quinoxalin-2-yl)propanamide (180 mg) and N-(6-aminoquinolin-5-yl)-3-(quinoxalin-2-yl)propanamide (80 mg) were isolated. MS (ESI) m/z 343 (M+H+).

後処理

  1. stirringthe reaction was stirred for 3 hours
  2. washThe mixture was washed with water (10 mL)
  3. extractionextracted with DCM (30 mL×3)
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto afford a yellow mixture which
  8. customwas purified by reverse phase chromatography

出典と根拠

ORDレコード
ord-7ebc2facb2034a4ea8a56b5956e90d7e
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969349B2

反応ノート

読み込み中…

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