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

HRID 1479147
ノート
印刷プレビュー

反応式

HRID 1479147 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 1

HCID 58641927
US10493060, Example BVD-523
収率 64%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-d15e9273037b40e196ef330a34eeda3c
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE046097E1

反応ノート

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