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Hydrochloric Acid → HCID 54054832, 화합물

HRID 1899790
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인쇄 미리보기

반응식

HRID 1899790 반응식
[C:1](=[O:6])([O:4][CH3:5])OC.[H-].[Na+].[CH3:9][C:10]1[CH:11]=[C:12]([CH:23]=[CH:24][CH:25]=1)[O:13][CH2:14][C:15]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=O.Cl.C1C[O:30]CC1>CO>[CH3:5][O:4][C:1](=[O:6])[CH2:18][C:19](=[O:30])[C:20]1[CH:21]=[CH:22][CH:17]=[CH:15][C:14]=1[O:13][C:12]1[CH:23]=[CH:24][CH:25]=[C:10]([CH3:9])[CH:11]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 12021Dimethyl CarbonateHCID 24758Sodium hydrideHCID 14970243alpha-(3-Methylphenoxy)acetophenone

생성물 1

HCID 54054832HCID 54054832, 화합물수율 93%

시약·촉매·용매 1

HCID 887
Methanol
용매

반응 조건

온도
50 °C

실험 절차

38.7 g (0.43 mol) of dimethyl carbonate are added to a suspension of 10.3 g (0.43 mol) of sodium hydride in 230 ml of THF and then, at 50° C., a solution of 67.2 g (0.30 mol) of 2-(3-methylphenoxy)acetophenone is added dropwise. The mixture is stirred at 50° C. for 3 hours, left to cool, 60 ml of methanol are added, and the mixture is stirred at room temperature overnight. It is acidified (pH 2) with 10 percent hydrochloric acid and extracted with MTB ether. The organic phase is washed with water, dried and concentrated. 79.5 g (93% yield) of methyl2-(3methylphenoxy)benzoylacetate remain as dark oil.

후처리

  1. waitleft
  2. temperatureto cool
  3. stirringthe mixture is stirred at room temperature overnight
  4. extractionextracted with MTB ether
  5. washThe organic phase is washed with water
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8b66d252261b474192a9386eb7c15834
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05573999

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