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 57920118、化合物

HRID 19186
ノート
印刷プレビュー

反応式

HRID 19186 の反応式
[OH:1][C@@H:2]([CH2:34]O)[CH2:3][N:4]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:33])[CH:11]([N:17]2[CH2:21][C:20]([O:22][C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH3:30])[C:24]=3[Cl:31])=[CH:19][C:18]2=[O:32])[CH2:12][C:13]([F:16])([CH3:15])[CH3:14])=[N:5]1.[CH3:36]N(C)CCCN=C=NCC.ON1C2C=CC=CC=2N=N1.Cl.O[C@@H](CO)CN1C=CC(NC(=O)[C@@H](N2CC(OC3C=CC=C(Cl)C=3Cl)=CC2=O)CC(C)C)=N1>ClCCl>[OH:1][C:2]([CH3:34])([CH3:36])[CH2:3][N:4]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:33])[CH:11]([N:17]2[CH2:21][C:20]([O:22][C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH3:30])[C:24]=3[Cl:31])=[CH:19][C:18]2=[O:32])[CH2:12][C:13]([F:16])([CH3:14])[CH3:15])=[N:5]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 579200982-[4-(2-Chloro-3-methoxyphenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-fluoro-4-methyl-pentanoic acid-[1-((R)-2,3-dihydroxy-propyl)-1H-pyrazol-3-yl]-amideHCID 66899094HMS5552 HCl

生成物 1

HCID 57920118HCID 57920118、化合物収率 57%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
25 °C

実験手順

A solution of 2-[4-(2-chloro-3-methoxy-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-fluoro-4-methyl-pentanoic acid (prepared as in Example 170, 200 mg, 0.54 mmol) in dichloromethane (20 mL) was treated with 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (92 mg, 0.59 mmol), 1-hydroxybenzotriazole (76 mg, 0.57 mmol) and 1-(3-amino-pyrazol-1-yl)-2-methyl-propan-2-ol (prepared in U.S. Pat. Appl. US2008021032 Example 80, 100 mg, 0.65 mmol). The reaction mixture was stirred for 18 h at 25° C., under nitrogen and then diluted with dichloromethane, washed with 2N hydrochloric acid, saturated sodium bicarbonate solution, a saturated sodium chloride solution and dried over magnesium sulfate. The crude product obtained after concentration, was purified by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 12 g; 0% to 10% methanol/dichloromethane) to afford 2-[4-(2-chloro-3-methoxy-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-fluoro-4-methyl-pentanoic acid [1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-yl]-amide (156 mg, 57%) as a white powder: LR-ES-MS m/z calculated for C24H30ClFN4O5 [M]+ 508, observed 509 [M+H]+; 1H NMR (300 MHz, DMSO-d6) δ ppm 1.05 (br. s., 3H), 1.06 (br. s., 3H), 1.19, 1.32 (2×d, J=3.0 Hz, 3H), 1.26, 1.39 (2×d, J=3.0 Hz, 3H), 1.96-2.33 (m, 2H), 3.90 (br. s., 5H), 4.25 (d, J=18.4 Hz, 1H), 4.52 (d, J=18.4 Hz, 1H), 4.67 (s, 1H), 4.77, 4.80 (2×s, 1H), 5.01, 5.10 (2×dd, J=9.8, 4.4 Hz, 1H), 6.44 (d, J=1.8 Hz, 1H), 7.00, 7.06 (2×d, J=8.2 Hz, 1H), 7.13 (d, J=8.2 Hz, 1H), 7.41 (t, J=8.2 Hz, 1H), 7.54 (d, J=1.8 Hz, 1H), 10.71, 10.82 (2×s, 1H).

後処理

  1. washwashed with 2N hydrochloric acid, saturated sodium bicarbonate solution
  2. dry with materiala saturated sodium chloride solution and dried over magnesium sulfate
  3. customThe crude product obtained
  4. concentrationafter concentration
  5. customwas purified by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 12 g; 0% to 10% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-383c9b006f234b6e816092bfdacb81a5
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07741327B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート