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Boron trifluoride etherate → HCID 24771803、化合物

HRID 2221429
ノート
印刷プレビュー

反応式

HRID 2221429 の反応式
[CH3:1][C:2]1([CH3:16])[C:6]([CH3:7])=[CH:5][CH2:4][CH:3]1[C:8]1[CH2:15][CH2:14][C:11]2([O:13][CH2:12]2)[CH2:10][CH:9]=1.B(F)(F)F.CCOCC>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:16])[C:6]([CH3:7])=[CH:5][CH2:4][CH:3]1[C:8]1[CH2:15][CH2:14][CH:11]([CH:12]=[O:13])[CH2:10][CH: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

4

反応物 2

HCID 8000Boron trifluoride etherateHCID 24771795HCID 24771795、化合物

生成物 1

HCID 24771803HCID 24771803、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

6-(2,2,3-Trimethyl-cyclopent-3-enyl)-1-oxa-spiro[2.5]oct-5-ene (XIV, 2.72 g, 12.5 mmol,), dissolved in toluene (5 ml), are added dropwise to a solution of BF3.OEt2 (1.7 ml) in toluene (20 ml). After 2 hours, the reaction solution is poured onto ice (10 ml), then the phases are separated and the organic phase is washed once with saturated NaCl solution. The organic phase is then dried over Na2SO4, filtered off and concentrated in a rotary evaporator. 2.07 g of crude product having a purity of 83% are obtained, which is used in the next step without being purified further.

後処理

  1. additionthe reaction solution is poured onto ice (10 ml)
  2. customthe phases are separated
  3. washthe organic phase is washed once with saturated NaCl solution
  4. dry with materialThe organic phase is then dried over Na2SO4
  5. filtrationfiltered off
  6. concentrationconcentrated in a rotary evaporator
  7. customare obtained
  8. customwithout being purified further

出典と根拠

ORDレコード
ord-a1da55a08e7b431a94ec83c6969e9544
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07368613B2

反応ノート

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