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

N-Isopropyl-2-[3-methyl-2,4-dioxo-5-phenyl-3-(3-phenyl-allyl)-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl]-N-phenyl acetamide → N-Isopropyl-2-[3-methyl-2,4-dioxo-5-phenyl-3-(3-phenyl-propyl)-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl]-N-phenyl acetamide

HRID 343198
ノート
印刷プレビュー

反応式

HRID 343198 の反応式
[CH:1]([N:4]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:5](=[O:36])[CH2:6][N:7]1[C:13](=[O:14])[C:12]([CH3:24])([CH2:15][CH:16]=[CH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:11](=[O:25])[N:10]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:9]2[CH:32]=[CH:33][CH:34]=[CH:35][C:8]1=2)([CH3:3])[CH3:2]>C(O)C.[Pd]>[CH:1]([N:4]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:5](=[O:36])[CH2:6][N:7]1[C:13](=[O:14])[C:12]([CH3:24])([CH2:15][CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:11](=[O:25])[N:10]([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[C:9]2[CH:32]=[CH:33][CH:34]=[CH:35][C:8]1=2)([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 67699497N-Isopropyl-2-[3-methyl-2,4-dioxo-5-phenyl-3-(3-phenyl-allyl)-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl]-N-phenyl acetamide

生成物 1

HCID 67700209N-Isopropyl-2-[3-methyl-2,4-dioxo-5-phenyl-3-(3-phenyl-propyl)-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl]-N-phenyl acetamide収率 0.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

To a stirring solution of 40 mg (71.7 mmol) of N-Isopropyl-2-[3-methyl-2,4-dioxo-5-phenyl-3-(3-phenyl-allyl)-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl]-N-phenyl acetamide, prepared as in Example 11, in 3 mL absolute ethanol is added 10 mg of 10% palladium on carbon. The reaction vessel is placed on a Parr hydrogenation apparatus, evacuated, and then pressurized with H2 gas to 40 psi and shaken for 2 h at RT. The reaction mixture is filtered through Celite to remove the catalyst and the solvent removed in vacuo. Purification of the resulting material via reverse phase MPLC using a C-18 column and 70% acetonitrile/30% H2O with 0.1% TFA as eluent followed by lyophilization afforded 29 mg of the title compound as a white amorphous solid: 1H NMR (CDCl3, 300 MHz) δ7.49-6.96 (m, 19H), 6.72 (d, 1H, J=8.0), 5.09 (m, 1H), 4.38 (d, 1H, J=16.3), 3.92 (d, 1H, J=16.3), 2.28 (m, 2H), 1.67-1.50 (m, 6H), 1.34 (m, 1H), 1.12 (m, 6H); low resolution MS (FAB)m/e 560 (MH+), 425, 397, 223.

後処理

  1. customevacuated
  2. filtrationThe reaction mixture is filtered through Celite
  3. customto remove the catalyst
  4. customthe solvent removed in vacuo
  5. customPurification of the resulting material via reverse phase MPLC

出典と根拠

ORDレコード
ord-8c188b648f8544de911b56e276320d89
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05859007

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