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

HRID 1754126노트

반응식

HRID 1754126 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-72efc72f5b424f1cb48cf501b41b280d
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169218B2

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