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Thionyl Chloride → 3-(2-chloroethyl)-2-phenylquinazolin-4(3H)-one

HRID 1156345
ノート
印刷プレビュー

反応式

HRID 1156345 の反応式
O[CH2:2][CH2:3][N:4]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]=[C:5]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.S(Cl)([Cl:23])=O>ClC(Cl)Cl>[Cl:23][CH2:2][CH2:3][N:4]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]=[C:5]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 8545423-(2-Hydroxyethyl)-2-phenyl-quinazolin-4-one

生成物 1

HCID 27720803-(2-chloroethyl)-2-phenylquinazolin-4(3H)-one

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a stirred mixture of 15 parts of 3-(2-hydroxyethyl)-2-phenyl-4(3H)-quinazolineone and 375 parts of trichloromethane are added dropwise 24 parts of thionyl chloride at room temperature. Upon completion, stirring is continued for 2 hours at reflux. The reaction mixture is evaporated. Water is added to the residue and the whole is neutralized with a sodium hydrogen carbonate solution. The product is extracted with trichloromethane. The extract is washed with water, dried, filtered and evaporated. The residue is crystallized from a mixture of 2,2'-oxybispropane and petroleumether. The product is filtered off and dried, yielding 11.6 parts of 3-(2-chloroethyl)-2-phenyl-4(3H)-quinazolinone.

後処理

  1. temperatureat reflux
  2. customThe reaction mixture is evaporated
  3. additionWater is added to the residue
  4. extractionThe product is extracted with trichloromethane
  5. washThe extract is washed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue is crystallized from a mixture of 2,2'-oxybispropane and petroleumether
  10. filtrationThe product is filtered off
  11. customdried

出典と根拠

ORDレコード
ord-6de35fc962be44e6a21e2ac5d8b0013b
出典データセット
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04335127

反応ノート

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