Chloroform → 3-(2-Chloroethyl)-2-ethyl-3,4-dihydro-4-quinazolinone

HRID 1028346ノート

反応式

HRID 1028346 の反応式
[CH2:1]([C:3]1[N:12]([CH2:13][CH2:14]O)[C:11](=[O:16])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]=1)[CH3:2].S(Cl)([Cl:19])=O.C(Cl)(Cl)Cl>CCCCCC>[Cl:19][CH2:14][CH2:13][N:12]1[C:11](=[O:16])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]=[C:3]1[CH2:1][CH3:2]

参加物

5

反応物 3

HCID 6212ChloroformHCID 24386Thionyl ChlorideHCID 103760834(3H)-Quinazolinone, 2-ethyl-3-(2-hydroxyethyl)-

生成物 1

HCID 597239043-(2-Chloroethyl)-2-ethyl-3,4-dihydro-4-quinazolinone収率 32.8%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

2-ethyl-3-(2-hydroxyethyl)quinazoline-4 (3H)-one (5.00 g; 22.91 mmol) and thionyl chloride (1.672 mL, 22.91 mmol) were added to a 150 mL reactor, together with 60 mL of chloroform. The reaction medium was heated to reflux and for completing the reaction, which was accompanied through CG/MS. After the end of the reaction, 100 mL of hexane were added and the solution was agitated at room temperature in order to precipitate the product. The resulting suspension was vacuum filtered, washed with two portions of hexane and dried, yielding 3-(2-chloroethyl)-2-ethylquinazoline-4 (3H)-one as a white solid (1.78 g; 7.52 mmol; yield: 32.8%).

後処理

  1. temperatureThe reaction medium was heated
  2. temperatureto reflux
  3. customthe reaction, which
  4. additionwere added
  5. customto precipitate the product
  6. filtrationfiltered
  7. washwashed with two portions of hexane
  8. customdried

出典と根拠

ORDレコード
ord-b05263fa38f14d76adbdb9be85e7eaa2
出典データセット
uspto-grants-2014_05
特許番号
US08735578B2

反応ノート

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