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-N-(4-methoxy-phenyl)-2-(2-phenylamino-phenylamino)-acetamide → 2-(3-Allyl-3-methoxy-2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl)-N-isopropyl-N-(4-methoxy-phenyl) acetamide

HRID 343093
ノート
印刷プレビュー

反応式

HRID 343093 の反応式
[CH2:1]([C:4]([O:11][CH3:12])([C:8](Cl)=[O:9])[C:5](Cl)=[O:6])[CH:2]=[CH2:3].[CH:13]([N:16]([C:34]1[CH:39]=[CH:38][C:37]([O:40][CH3:41])=[CH:36][CH:35]=1)[C:17](=[O:33])[CH2:18][NH:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[NH:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)([CH3:15])[CH3:14]>C1COCC1>[CH2:1]([C:4]1([O:11][CH3:12])[C:8](=[O:9])[N:19]([CH2:18][C:17]([N:16]([CH:13]([CH3:15])[CH3:14])[C:34]2[CH:39]=[CH:38][C:37]([O:40][CH3:41])=[CH:36][CH:35]=2)=[O:33])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[N:26]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:5]1=[O:6])[CH:2]=[CH2:3]
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 2

HCID 10644060N-Isopropyl-N-(4-methoxy-phenyl)-2-(2-phenylamino-phenylamino)-acetamideHCID 542245772-Allyl-2-methoxy-propandioyl dichloride

生成物 1

HCID 676965942-(3-Allyl-3-methoxy-2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl)-N-isopropyl-N-(4-methoxy-phenyl) acetamide収率 58.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirring solution of 1.50 g (7.10 mmol) of 2-allyl-2-methoxy-propandioyl dichloride in 50 mL of THF at 0° C. is added dropwise over 2 min a solution of 1.85 g (4.74 mmol) of N-isopropyl-N-(4-methoxy-phenyl)-2-(2-phenylamino-phenylamino) acetamide, prepared as in Intermediate 43, in 20 mL of THF. The resulting solution is stirred at RT for 15 min then refluxed for 18 h. After cooling to RT the solvent is removed in vacuo and the crude product purified by silica gel flash column chromatography using hexane/EtOAc 3/1 as eluent to afford 1.46 g of the title compound as a clear, colorless oil: 1H NMR (CDCl3, 300 MHz) δ7.40-6.88 (m, 12H), 6.78 (d, 1H), 5.92 (m, 1H), 5.10 (m, 2H), 4.46 (d, 1H), 3.80 (s, 3H), 3.64 (m, 1H), 3.02 (s, 3H), 1.88 (m, 1H), 1.75 (m, 1H), 1.13 (m, 6H); low resolution MS (FAB) m/e 528 (MH+).

後処理

  1. temperaturethen refluxed for 18 h
  2. temperatureAfter cooling to RT the solvent
  3. customis removed in vacuo
  4. customthe crude product purified by silica gel flash column chromatography

出典と根拠

ORDレコード
ord-4f675bba60e2446db996971389516c17
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