ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 178492636、化合物

HRID 420135
ノート
印刷プレビュー

反応式

HRID 420135 の反応式
[CH:1]1([N:4]2[C:12]3[C:7](=[C:8]([O:16][CH3:17])[CH:9]=[C:10]([C:13]([OH:15])=O)[CH:11]=3)[CH:6]=[CH:5]2)[CH2:3][CH2:2]1.[O:18]=[C:19]1[C:33]2[C:28](=[CH:29][CH:30]=[C:31]([C:34]3[NH:35][C:36]([C:39]([NH2:41])=[O:40])=[N:37][N:38]=3)[CH:32]=2)[O:27][C:21]2([CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH2:20]1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C>CN(C=O)C.O>[CH:1]1([N:4]2[C:12]3[C:7](=[C:8]([O:16][CH3:17])[CH:9]=[C:10]([C:13]([N:24]4[CH2:23][CH2:22][C:21]5([CH2:20][C:19](=[O:18])[C:33]6[C:28](=[CH:29][CH:30]=[C:31]([C:34]7[NH:35][C:36]([C:39]([NH2:41])=[O:40])=[N:37][N:38]=7)[CH:32]=6)[O:27]5)[CH2:26][CH2:25]4)=[O:15])[CH:11]=3)[CH:6]=[CH:5]2)[CH2:2][CH2:3]1
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 666494031-cyclopropyl-4-methoxy-1H-indole-6-carboxylic acidHCID 178513836HCID 178513836、化合物

生成物 1

HCID 178492636HCID 178492636、化合物

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-cyclopropyl-4-methoxy-1H-indole-6-carboxylic acid (54 mg) and 5-[4-oxo-spiro(chroman-2,4′-piperidin)-6-yl]-4H-1,2,4-triazole-3-carboxamide (102 mg) in DMF (4 mL) were added TEA (77 uL), HOBT (42 mg), and WSC (53 mg) at room temperature and the reaction mixture was stirred at room temperature overnight. The reaction mixture was poured into H2O, extracted with CHCl3, dried over sodium sulfate, filtered, and concentrated in reduced pressure. The residue was purified by column chromatography on silica gel using a mixture of CHCl3/MeOH (1:0-10:1) as eluent to give the title compound as a colorless solid. 1H-NMR (400 MHz, CDCl3) δ: 8.78-8.60 (1H, m), 8.40-8.25 (1H, m), 7.29 (1H, s), 7.15 (1H, d, J=8.0 Hz), 7.09 (1H, d, J=4.0 Hz), 6.57 (1H, s), 6.52 (1H, d, J=4.0 Hz), 4.30-4.17 (1H, m), 3.95 (3H, s), 3.62-3.38 (3H, m), 3.38-3.32 (1H, m), 2.85 (2H, s), 2.28-1.70 (4H, m), 1.06-1.04 (2H, m), 1.00-0.97 (2H, m); MS [M+H]+=541.

後処理

  1. extractionextracted with CHCl3
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in reduced pressure
  5. customThe residue was purified by column chromatography on silica gel using
  6. additiona mixture of CHCl3/MeOH (1:0-10:1) as eluent

出典と根拠

ORDレコード
ord-b4339f12e0aa4de497549e82acd6dc88
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08093389B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート