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Triethylamine → 4,4-Dimethyl-6-trimethylsilanyl-ethynyl-1,2,3,4-tetrahydronaphthalene-1-one

HRID 51632
ノート
印刷プレビュー

反応式

HRID 51632 の反応式
[CH3:1][C:2]1([CH3:21])[C:11]2[C:6](=[CH:7][CH:8]=[C:9](OS(C(F)(F)F)(=O)=O)[CH:10]=2)[C:5](=[O:20])[CH2:4][CH2:3]1.[CH3:22][Si:23](C#C)([CH3:25])[CH3:24].[CH2:28](N(CC)CC)[CH3:29]>O1CCCC1.C(OCC)C.[Cu]I.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>[CH3:1][C:2]1([CH3:21])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Si:23]([CH3:25])([CH3:24])[CH3:22])[CH:10]=2)[C:5](=[O:20])[CH:4]([C:28]#[CH:29])[CH2:3]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

8

反応物 3

HCID 8471TriethylamineHCID 66111TrimethylsilylacetyleneHCID 225687874,4-Dimethyl-6-trifluoromethylsulfonyloxy-1,2,3,4-tetrahydronaphthalene-1-one2 回

生成物 1

HCID 865859204,4-Dimethyl-6-trimethylsilanyl-ethynyl-1,2,3,4-tetrahydronaphthalene-1-one収率 72%

試薬・触媒・溶媒 4

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 178418476HCID 178418476、化合物触媒
HCID 3283Diethyl Ether溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

A solution of 4,4-dimethyl-6-trifluoromethylsulfonyloxy-1,2,3,4-tetrahydronaphthalene-1-one (Intermediate 11, 0.46 g, 1.43 mmol) in triethyl amine (3 mL) and anhydrous tetrahydrofuran (8 mL) was treated with copper(I)iodide (0.1 g, 0.53 mmol) and sparged with argon for 5 minutes. Trimethylsilyl acetylene (0.85 mL, 6 mmol) was then added followed by dichlorobis(triphenylphosphine)palladium(II) (0.25 g, 0.36 mmol). The resulting reaction mixture was heated at 70° C. for 17 h. It was then cooled to ambient temperature, diluted with diethyl ether and filtered over a bed of celite. The filtrate was evaporated vacuo to an oil which was subjected to flash column chromatography over silica gel (230-400 mesh) using 5% ethyl acetate in hexane as the eluent to afford the title compound (0.28 g, 72%).

後処理

  1. customsparged with argon for 5 minutes
  2. customThe resulting reaction mixture
  3. temperatureIt was then cooled to ambient temperature
  4. filtrationfiltered over a bed of celite
  5. customThe filtrate was evaporated vacuo to an oil which

出典と根拠

ORDレコード
ord-5300da80c1114a449dd9b59d2bf98669
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06713647B2

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