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Ethyl 4-iodobenzoate → Ethyl 4-[(2,2-dimethyl-4-oxo-chroman-6-yl)ethynyl]-benzoate

HRID 619649
ノート
印刷プレビュー

反応式

HRID 619649 の反応式
[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][C:8]([CH3:14])([CH3:13])[CH2:7][C:6]2=[O:15])#[CH:2].I[C:17]1[CH:27]=[CH:26][C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:19][CH:18]=1>CCN(CC)CC.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I>[CH3:14][C:8]1([CH3:13])[CH2:7][C:6](=[O:15])[C:5]2[C:10](=[CH:11][CH:12]=[C:3]([C:1]#[C:2][C:17]3[CH:27]=[CH:26][C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:19][CH:18]=3)[CH:4]=2)[O:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 142891Ethyl 4-iodobenzoateHCID 218466816-Ethynyl-2,2-dimethylchroman-4-one2 回

生成物 1

HCID 21846646Ethyl 4-[(2,2-dimethyl-4-oxo-chroman-6-yl)ethynyl]-benzoate収率 50.3%

試薬・触媒・溶媒 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 178418476
HCID 178418476、化合物
触媒
HCID 8471Triethylamine溶媒

実験手順

A solution of 6-ethynyl-2,2-dimethylchroman-4-one (Compound 262, 2.60 g, 13.0 mmol) and ethyl 4-iodobenzoate (3.6 g, 13.0 mmol) in 50.0 mL Et3N was purged with argon for 15 minutes. To this solution was added bis(triphenylphosphine)-palladium(II) chloride (1.82 g, 2.6 mmol) and copper(I) iodide (496 mg, 2.6 mmol). After sparging for an additional 10 minutes with argon, the solution was stirred overnight at room temperature. The reaction mixture was filtered through a pad of Celite using an Et2O wash. Concentration of the filtrate under reduced pressure, followed by column chromatography (2-5% EtOAc-hexanes) of the residual solid afforded 2.28 g (50%) the title compound as an orange solid. 1H NMR (300 MHz, CDCl3) δ: 8.06 (1H, d, J=2.2 Hz), 8.02 (2H, d, J=8.5 Hz), 2.61 (1H, dd, J=2.2, 8.6 Hz), 7.55 (2H, d, J=8.5 Hz), 6.93 (1H, d, J=8.6 Hz), 4.39 (2H, q, J=7.1 Hz), 2.75 (3H, s), 1.48 (6H, s), 1.41 (t, J=7.1 Hz).

後処理

  1. customAfter sparging for an additional 10 minutes with argon
  2. filtrationThe reaction mixture was filtered through a pad of Celite
  3. washwash

出典と根拠

ORDレコード
ord-ee19218a55e14a52a9edeb3e485bc7c7
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05958954

反応ノート

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