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

HRID 1754126ノート

反応式

HRID 1754126 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-72efc72f5b424f1cb48cf501b41b280d
出典データセット
uspto-grants-2015_10
特許番号
US09169218B2

反応ノート

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