Carbon Tetrachloride → 1-Chloromethyl-4-prop-2-ynyloxymethyl-benzene
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
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
- temperatureunder reflux
- concentrationafter which the reaction mixture was concentrated under a reduced pressure
- 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
反応ノート
読み込み中…