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Potassium Carbonate → HCID 12881313, 화합물

HRID 745513
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HRID 745513 반응식
[CH3:1][CH:2]([C:4]1[CH:5]=[C:6]2[C:11](=[C:12]([CH:14]([CH3:16])[CH3:15])[CH:13]=1)[N:10]=[CH:9][NH:8][C:7]2=[O:17])[CH3:3].[CH3:18][O:19][C:20](=[O:24])/[CH:21]=[CH:22]\Cl.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:18][O:19][C:20](=[O:24])/[CH:21]=[CH:22]/[N:8]1[C:7](=[O:17])[C:6]2[C:11](=[C:12]([CH:14]([CH3:16])[CH3:15])[CH:13]=[C:4]([CH:2]([CH3:1])[CH3:3])[CH:5]=2)[N:10]=[CH:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 5352274Methyl cis-3-chloropropenoateHCID 136147100HCID 136147100, 화합물

생성물 1

HCID 12881313HCID 12881313, 화합물수율 74%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 3.10 g (0.013)mol) of 6,8-bis-(1-methylethyl)-quinazolin-4(3H)-one, 1.78 g (0.0148 mol) of (Z)-3-chloro-2-propenoic acid methyl ester and 3.72 g (0.027 mol) of anhydrous potassium carbonate in 100 ml. of anhydrous acetone was stirred at reflux for 17 hr. The reaction mixture was filtered, the solid was washed with acetone and the filtrate was concentrated in vacuo to an oil which soon crystallized. Recrystallization from methanol gave 3.11 g, m.p. 102°-103°, (74% yield) of (E)-3-[6,8-bis-(1-methylethyl)-4-oxo-4H-quinazolin-3-yl]-2-propenoic acid methyl ester.

후처리

  1. temperatureat reflux for 17 hr
  2. filtrationThe reaction mixture was filtered
  3. washthe solid was washed with acetone
  4. concentrationthe filtrate was concentrated in vacuo to an oil which
  5. customsoon crystallized
  6. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-cb2139f2827641c5b8f726687c09c2b6
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04599336

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