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

HRID 520286노트

반응식

HRID 520286 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-68c1ffa6ddc34379bd6fe87116192aab
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09326984B2

반응 노트

불러오는 중…