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Triphenylphosphine → HCID 68408471、化合物

HRID 1176175
ノート
印刷プレビュー

反応式

HRID 1176175 の反応式
I[C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[C:5](I)=[CH:4][C:3]=1[O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].C1C=CC(P([C:40]2[CH:45]=CC=CC=2)C2C=CC=CC=2)=CC=1.[CH3:46][Si:47]([C:50]#[CH:51])([CH3:49])[CH3:48]>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.N1CCCCC1>[CH3:46][Si:47]([C:50]#[C:51][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[C:5]([C:40]#[C:45][Si:47]([CH3:49])([CH3:48])[CH3:46])=[CH:4][C:3]=1[O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])([CH3:49])[CH3:48]
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 3

HCID 11776TriphenylphosphineHCID 66111TrimethylsilylacetyleneHCID 113192531,4-Diiodo-2,5-bis(octyloxy)benzene

生成物 1

HCID 68408471HCID 68408471、化合物

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 8082Piperidine溶媒

反応条件

温度
60 °C

実験手順

1,4-Diiodo-2,5-di-n-octyloxybenzene (4.01 g, 6.84×10−3 mol), Pd(PPh3)2Cl2 (0.248 g, 3.53×10−4 mol), PPh3 (0.179 g, 6.82×10−4 mol), CuI (0.072 g, 3.8×10−4 mol) and piperidine (40 ml) were added to a 100-ml round-bottom flask. Ar was bubbled into the reaction mixture for 5 min before trimethylsilylacetylene (3.0 ml, 2.1×10−2 mol) was added. The reaction mixture was stirred at 60° C. for 2 h under Ar. After cooling, the solvent was evaporated. CHCl3 was added to the residue, and the organic solution was washed with aqueous NH4Cl (3 times), water, and dried over Na2SO4. After the solvent was evaporated, the residue was chromatographed on silica gel with 2:1 hexane:CHCl3 as the eluent. Yield=3.455 g (96% based on 4.01 g of 1,4-diiodo-2,5-di-n-octyloxybenzene). 1H NMR (300 MHz, CDCl3): δ 6.88 (s, 2H, Ph-H), 3.94 (t, 4H, J=6.4 Hz, —OCH2), 1.78 (quint, 4H, J=6.9 Hz, —OCH2CH2—), 1.42-1.60 (m, 4H, —OCH2CH2CH2—), 1.16-1.42 (m, 16H, —CH2—), 0.88 (t, 6H, J=6.7 Hz, —CH3), 0.25 (s, 18H, —Si—CH3). CI MS m/z: 526.366 (M+) (calcd 526.366).

後処理

  1. additionwas added
  2. temperatureAfter cooling
  3. customthe solvent was evaporated
  4. additionCHCl3 was added to the residue
  5. washthe organic solution was washed with aqueous NH4Cl (3 times), water
  6. dry with materialdried over Na2SO4
  7. customAfter the solvent was evaporated
  8. customthe residue was chromatographed on silica gel with 2:1 hexane

出典と根拠

ORDレコード
ord-f874ca03d87f44269c09f5291c7f21eb
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842758B2

反応ノート

読み込み中…

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