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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → US10493060, Example BVD-523

HRID 1479147
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HRID 1479147 반응식
[Cl:1][C:2]1[C:3]([C:12]2[CH:13]=[C:14]([C:17]([OH:19])=O)[NH:15][CH:16]=2)=[CH:4][C:5]([NH:8][CH:9]([CH3:11])[CH3:10])=[N:6][CH:7]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH:41]1[CH:46]=[C:45]([Cl:47])[CH:44]=[C:43]([C@H:48]([NH2:51])[CH2:49][OH:50])[CH:42]=1.C(N(C(C)C)CC)(C)C>CN(C=O)C.O>[Cl:47][C:45]1[CH:44]=[C:43]([CH:48]([NH:51][C:17]([C:14]2[NH:15][CH:16]=[C:12]([C:3]3[C:2]([Cl:1])=[CH:7][N:6]=[C:5]([NH:8][CH:9]([CH3:10])[CH3:11])[CH:4]=3)[CH:13]=2)=[O:19])[CH2:49][OH:50])[CH:42]=[CH:41][CH:46]=1
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참가 물질

8

반응물 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 586419264-(5-chloro-2-(isopropylamino)pyridin-4-yl)-1H-pyrrole-2-carboxylic acidHCID 59694427(S)-2-amino-2-(3-chlorophenyl)ethanol

생성물 1

HCID 58641927
US10493060, Example BVD-523
수율 64%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 4-(5-chloro-2-isopropylaminopyridin-4-yl)-1H-pyrrole-2-carboxylic acid (1.93 g, 6.9 mmol, 1.0 equivalent) in DMF (5.0 mL) was added EDCI (1.45 g, 7.6 mmol, 1.1 equivalents), HOBt (0.94 g, 6.9 mmol, 1.0 equivalent) and (S)-3-chlorophenylglycynol (1.58 g, 7.6 mmol, 1.1 equivalents). Diisopropylethylamine (2.7 mL) was then added and the resulting mixture was stirred a room temperature overnight. The mixture was then poured into water and extracted with ethyl acetate. After drying over sodium sulfate, the solvent was removed and the crude was adsorbed on silica gel. Purification was effected by flash chromatography on silica, eluting with mixtures of hexanes/acetone (from 80:20 to 60:40) to afford the title compound as white solid (1.9 g, 64%). Rt(min) 4.981 s. FIA MS: 433.1 ES+; 431.2 ES−. 1HNMR (CD3OD) δ 1.31 (d, 6H), 3.85 (m, 3H), 5.15 (t, 1H), 7.01 (s, 1H), 7.25 (m, 3H), 7.4 (s, 1H), 7.45 (s, 1H), 7.7 (s, 1H), 7.95 (s, 1H).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialAfter drying over sodium sulfate
  3. customthe solvent was removed
  4. customPurification
  5. washeluting with mixtures of hexanes/acetone (from 80:20 to 60:40)

출처 및 근거

ORD 기록
ord-d15e9273037b40e196ef330a34eeda3c
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE046097E1

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