Thionyl Chloride → 2-Chloromethyl-5,6,7-trimethoxynaphthalene

HRID 720303ノート

反応式

HRID 720303 の反応式
O[CH2:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][C:7]([O:17][CH3:18])=[C:8]([O:15][CH3:16])[C:9]=2[O:13][CH3:14])[CH:4]=1.S(Cl)([Cl:21])=O.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[Cl:21][CH2:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][C:7]([O:17][CH3:18])=[C:8]([O:15][CH3:16])[C:9]=2[O:13][CH3:14])[CH:4]=1

参加物

5

反応物 3

HCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 218915782-Hydroxymethyl-5,6,7-trimethoxynaphthalene

生成物 1

HCID 218916422-Chloromethyl-5,6,7-trimethoxynaphthalene

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

2-Hydroxymethyl-5,6,7-trimethoxynaphthalene (781 mg) was dissolved in chloroform (6 mL), and thionyl chloride (561 mL) was added dropwise to the solution. After stirring at room temperature for 5 hours, the reaction mixture was poured into ice water, and sodium hydrogencarbonate was added to adjust the pH of the reaction mixture to 8 to conduct extraction with ethyl acetate. The resultant organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain the title compound.

後処理

  1. additionwas added
  2. extractionextraction with ethyl acetate
  3. washThe resultant organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-55f8372451644e1b8dd629ed599d8b66
出典データセット
uspto-grants-2006_11
特許番号
US07135473B2

反応ノート

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