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

HRID 258906

반응식

HRID 258906 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. Upo 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. stirringUpo 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-d3ee408cef0547e2b531a9f6a606d6c8
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035376

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