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

Triethylamine → Tert-butyl 4-[2-(4-(2-phenylethenyl)-3-pyridyl)ethynyl]benzoate

HRID 1106834
ノート
印刷プレビュー

反応式

HRID 1106834 の反応式
Br[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=[CH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[C:16]([C:18]1[CH:30]=[CH:29][C:21]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])=[CH:20][CH:19]=1)#[CH:17].C(N(CC)CC)C>CN(C=O)C.[Cu](I)(I)I>[C:10]1([CH:9]=[CH:8][C:7]2[CH:6]=[CH:5][N:4]=[CH:3][C:2]=2[C:17]#[C:16][C:18]2[CH:30]=[CH:29][C:21]([C:22]([O:24][C:25]([CH3:26])([CH3:28])[CH3:27])=[O:23])=[CH:20][CH:19]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=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 3

HCID 8471TriethylamineHCID 13965008Tert-butyl 4-ethynylbenzoateHCID 539315873-Bromo-4-(2-phenylethenyl)pyridine

生成物 1

HCID 54016878Tert-butyl 4-[2-(4-(2-phenylethenyl)-3-pyridyl)ethynyl]benzoate収率 33%

試薬・触媒・溶媒 2

HCID 178506583HCID 178506583、化合物触媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
95 °C

実験手順

3-Bromo-4-(2-phenylethenyl)pyridine (0.74 g, 2.9 mmol) was dissolved in DMF (1.4 ml). The solution was treated with tert-butyl 4-ethynylbenzoate (0.93 g, 4.6 mmol), copper (III) iodide (0.023 g, 0.21 mmol) and triethylamine (0.64 g, 6.3 mmol). The reaction mixture was degassed by bubbling through argon and the catalyst, bistriphenyl phosphinepalladium dichloride (0.03 g, 0.043 mmol), was added. The reaction was heated to 90-100° C. for 3 hours and then partitioned between ethyl acetate and water. The organic layer was washed with water (3×), dried (MgSO4) and evaporated. The residue was purified by chromatography (eluting with ethylacetate/hexane) to give tert-butyl 4-[2-(4-(2-phenylethenyl)-3-pyridyl)ethynyl]benzoate as a dark oil (0.36 g, 33%).

後処理

  1. customThe reaction mixture was degassed
  2. customby bubbling through argon
  3. additionthe catalyst, bistriphenyl phosphinepalladium dichloride (0.03 g, 0.043 mmol), was added
  4. custompartitioned between ethyl acetate and water
  5. washThe organic layer was washed with water (3×)
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. customThe residue was purified by chromatography (eluting with ethylacetate/hexane)

出典と根拠

ORDレコード
ord-75a8a525e6174f8c9d0c05e1e0adb425
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06057345

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