Thionyl Chloride → HCID 10035354、化合物

HRID 1534419ノート

反応式

HRID 1534419 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH2:5][CH2:6]O.S(Cl)([Cl:15])=O>C(Cl)Cl>[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH2:5][CH2:6][Cl:15]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 100349915-(2-Hydroxyethyl)-2-methoxyphenol

生成物 1

HCID 10035354HCID 10035354、化合物収率 33%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3-hydroxy-4-methoxyphenethyl alcohol (2.25 g) and thionyl chloride (5 ml) in methylene chloride (120 ml) was heated under reflux for 16 hours and evaporated. The residue was azeotroped twice with hexane and purified by chromatography on silica (30 g) using methylene chloride plus 0-6% methanol as the eluant. Appropriate fractions were combined and evaporated to give the title compound as a colourless solid (0.82 g, 33%), m.p. 53°-54°, which was characterised by its 1H-n.m.r. spectrum.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. customevaporated
  4. customThe residue was azeotroped twice with hexane
  5. custompurified by chromatography on silica (30 g)
  6. customevaporated

出典と根拠

ORDレコード
ord-56d2b0da3af145f2a526f46e6ee93563
出典データセット
uspto-grants-1992_02
特許番号
US05089505

反応ノート

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