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

HRID 1439558

反応式

HRID 1439558 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6f9f240ca6b442e68d5674a0bf10a51c
出典データセット
uspto-grants-1977_11
特許番号
US04060528

関連ノート

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