Carbon Tetrachloride → 1-Chloromethyl-4-prop-2-ynyloxymethyl-benzene

HRID 78208

反応式

HRID 78208 の反応式
[CH2:1]([O:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12]O)=[CH:8][CH:7]=1)[C:2]#[CH:3].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:34]>>[Cl:34][CH2:12][C:9]1[CH:10]=[CH:11][C:6]([CH2:5][O:4][CH2:1][C:2]#[CH:3])=[CH:7][CH:8]=1

参加物

4

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 545201314-[(2-Propynyloxy)methyl]benzyl alcohol

生成物 1

HCID 592552251-Chloromethyl-4-prop-2-ynyloxymethyl-benzene収率 84%

実験手順

A mixture of (4-prop-2-ynyloxymethyl-phenyl)-methanol (190 mg, 1.1 mmol) described in Manufacturing Example 194-1-1, triphenylphosphine (340 mg, 1.3 mmol), and carbon tetrachloride (3 mL) was stirred for 6 hours under reflux. The reaction mixture was cooled to room temperature, after which the reaction mixture was concentrated under a reduced pressure. The residue was purified by neutral silica gel column chromatography (ethyl acetate:heptane=1:10) to obtain the title compound (180 mg, 84%).

後処理

  1. temperatureunder reflux
  2. concentrationafter which the reaction mixture was concentrated under a reduced pressure
  3. customThe residue was purified by neutral silica gel column chromatography (ethyl acetate:heptane=1:10)

出典と根拠

ORDレコード
ord-4dddc4e094574863ae13f36a6f3e1418
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

関連ノート

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