Carbon Tetrachloride → HCID 59759003、化合物

HRID 914484ノート

反応式

HRID 914484 の反応式
[CH3:1][O:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11]O)=[CH:7][CH:6]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:33]>>[Cl:33][CH2:11][C:8]1[CH:9]=[CH:10][C:5]([CH2:4][CH2:3][O:2][CH3:1])=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 59759121886531-77-7

生成物 1

HCID 59759003HCID 59759003、化合物

実験手順

[4-(2-Methoxyethyl)phenyl]methanol (415 mg) synthesized in Reference Example 42 was dissolved in carbon tetrachloride (8 mL), triphenylphosphine (720 mg) was added thereto, and the mixture was heated under reflux for 4 hr. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in hexane, the insoluble material was filtered off, and the filtrate was evaporated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=20:1) to give the title compound (225 mg) as a colorless oil.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in hexane
  5. filtrationthe insoluble material was filtered off
  6. customthe filtrate was evaporated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=20:1)

出典と根拠

ORDレコード
ord-8e51b95470514f07988902eac63c54b0
出典データセット
uspto-grants-2011_09
特許番号
US08026370B2

反応ノート

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