Thionyl Chloride → alpha-Chloro-p-tolyl 2-thienyl ketone

HRID 461718

반응식

HRID 461718 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14]O)=[CH:10][CH:9]=1)=[O:7].S(Cl)([Cl:18])=O>C1C=CC=CC=1>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][Cl:18])=[CH:10][CH:9]=1)=[O:7]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 21391792alpha-Hydroxy-p-tolyl 2-thienyl ketone

생성물 1

HCID 21391736alpha-Chloro-p-tolyl 2-thienyl ketone

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a stirred and cooled suspension of 31 parts of α-hydroxy-p-tolyl 2-thienyl ketone in 160 parts of dry benzene are added dropwise 24 parts of thionyl chloride at 10° C. Upon completion, stirring is continued overnight at room temperature. The reaction mixture is evaporated and the residue is evaporated twice more from toluene. The latter residue is triturated in petroleumether. The product is filtered off and dissolved in 320 parts of ether. This solution is stirred with charcoal, filtered and the filtrate is evaporated. The residue is crystallized from ethanol at -20° C, yielding α-chloro-p-tolyl 2 -thienyl ketone.

후처리

  1. temperaturecooled
  2. stirringUpon completion, stirring
  3. customThe reaction mixture is evaporated
  4. customthe residue is evaporated twice more from toluene
  5. customThe latter residue is triturated in petroleumether
  6. filtrationThe product is filtered off
  7. dissolutiondissolved in 320 parts of ether
  8. stirringThis solution is stirred with charcoal
  9. filtrationfiltered
  10. customthe filtrate is evaporated
  11. customThe residue is crystallized from ethanol at -20° C

출처 및 근거

ORD 기록
ord-0a63a6d00ba049ebbac099dcd1dee036
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04064132

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