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,N'-Dimethylethylenediamine → 2-Bromo-6-(5-tert-butyl-1-oxoisoindolin-2-yl)benzyl Acetate

HRID 872148
ノート
印刷プレビュー

反応式

HRID 872148 の反応式
[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[NH:9][CH2:8]2)([CH3:4])([CH3:3])[CH3:2].[C:15]([O:18][CH2:19][C:20]1[C:25]([Br:26])=[CH:24][CH:23]=[CH:22][C:21]=1Br)(=[O:17])[CH3:16].C(=O)([O-])[O-].[Cs+].[Cs+].CNCCNC>[Cu](I)I.O1CCOCC1>[C:15]([O:18][CH2:19][C:20]1[C:21]([N:9]2[CH2:8][C:7]3[C:11](=[CH:12][CH:13]=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH:6]=3)[C:10]2=[O:14])=[CH:22][CH:23]=[CH:24][C:25]=1[Br:26])(=[O:17])[CH3:16]
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

7

反応物 4

HCID 8070N,N'-DimethylethylenediamineHCID 10796Cesium carbonateHCID 576339115-(Tert-butyl)isoindolin-1-oneHCID 592164132,6-Dibromobenzyl acetate

生成物 1

HCID 866979352-Bromo-6-(5-tert-butyl-1-oxoisoindolin-2-yl)benzyl Acetate収率 44.1%

試薬・触媒・溶媒 2

HCID 83717
Copper iodide
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
105 °C

実験手順

A 100-mL three-neck round-bottomed flask equipped with a reflux condenser, magnetic stirrer was purged with nitrogen and charged with 102c (570 mg, 3.02 mmol), 102d (1.85 g, 6.04 mmol), cesium carbonate (1.96 g, 6.04 mmol), N,N′-dimethyl-ethylenediamine (266 mg, 3.02 mmol), and 1,4-dioxane (27 mL). After bubbling nitrogen through the resulting suspension for 30 min, copper iodide (287 mg, 1.51 mmol) was added, and the reaction mixture was heated at 105° C. (oil bath temperature) for 14 h. After this time, the mixture was cooled to room temperature and filtered. The filtrate was diluted with ethyl acetate (150 mL) and water (30 mL). The organic layer was separated, and the aqueous layer was extracted with ethyl acetate (3×50 mL). The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (silica, 0% to 50% ethyl acetate/hexanes) to afford a 41% yield (555 mg) of 102e as an off-white solid: mp 176-178° C.; 1H NMR (300 MHz, CDCl3) δ 7.86 (d, 1H, J=8.1 Hz), 7.66 (dd, 1H, J=7.9, 1.5 Hz), 7.59 (dd, 1H, J=8.1, 1.5 Hz), 7.52 (s, 1H), 7.29 (m, 2H), 5.20 (s, 2H), 4.77 (s, 2H), 1.99 (s, 3H), 1.40 (s, 9H); MS (ESI+) m/z 416.1 (M+H).

後処理

  1. customA 100-mL three-neck round-bottomed flask equipped with a reflux condenser, magnetic stirrer
  2. customwas purged with nitrogen
  3. customAfter bubbling nitrogen through the resulting suspension for 30 min
  4. temperatureAfter this time, the mixture was cooled to room temperature
  5. filtrationfiltered
  6. additionThe filtrate was diluted with ethyl acetate (150 mL) and water (30 mL)
  7. customThe organic layer was separated
  8. extractionthe aqueous layer was extracted with ethyl acetate (3×50 mL)
  9. dry with materialThe combined organic layers were dried over sodium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by column chromatography (silica, 0% to 50% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-4447f935effe4ec787d8f6833ec95ca4
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08975260B2

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