Thionyl Chloride → HCID 10035354, 화합물

HRID 1534419노트

반응식

HRID 1534419 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 10035354HCID 10035354, 화합물수율 33%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-56d2b0da3af145f2a526f46e6ee93563
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05089505

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