Carbon Tetrachloride → 1-(Chloromethyl)-4-phenoxybenzene

HRID 77872

反応式

HRID 77872 の反応式
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14]O)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:36]>>[Cl:36][CH2:14][C:11]1[CH:12]=[CH:13][C:8]([O:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:9][CH:10]=1

参加物

4

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 826195(4-Phenoxyphenyl)methanol

生成物 1

HCID 5209941-(Chloromethyl)-4-phenoxybenzene収率 92%

実験手順

To a solution of (4-phenoxy-phenyl)-methanol (408 mg, 2.04 mmol) in carbon tetrachloride (8.2 mL) was added triphenylphosphine (642 mg, 2.45 mmol) under nitrogen atmosphere at room temperature, and the reaction solution was stirred under reflux for 7 hours and 40 minutes. The reaction mixture was cooled to room temperature and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=10:1) to obtain the title compound (409 mg, 92%).

後処理

  1. temperatureunder reflux for 7 hours and 40 minutes
  2. concentrationconcentrated under a reduced pressure
  3. customThe residue was purified by silica gel column chromatography (heptane:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-2670389cf36c4c69b06d1af2d077ee02
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

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