Calcium Carbonate → 6-[3-[4-(1-Pyrrolidinyl)phenyl]propoxy]-2-hexanone

HRID 1721965노트

반응식

HRID 1721965 반응식
[CH3:1][C:2]1([CH2:8][CH2:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([N:22]3[CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:18][CH:17]=2)SCCCS1.C(=O)([O-])[O-:28].[Ca+2]>C1COCC1.CO.O.[Hg](Cl)Cl>[N:22]1([C:19]2[CH:20]=[CH:21][C:16]([CH2:15][CH2:14][CH2:13][O:12][CH2:11][CH2:10][CH2:9][CH2:8][C:2](=[O:28])[CH3:1])=[CH:17][CH:18]=2)[CH2:26][CH2:25][CH2:24][CH2:23]1

참가 물질

6

반응물 2

HCID 10112Calcium CarbonateHCID 198627331-[4-[3-[4-(2-Methyl-1,3-dithian-2-yl)butoxy]propyl]phenyl]pyrrolidine

생성물 1

HCID 198627016-[3-[4-(1-Pyrrolidinyl)phenyl]propoxy]-2-hexanone

시약·촉매·용매 3

HCID 24085Mercuric Chloride촉매HCID 8028Tetrahydrofuran용매HCID 22242641Methanol--water (1/1)용매

실험 절차

A solution of the product of stage (iv) (3.2 g) in THF (50 ml) was added to a stirred suspension of mercury (II) chloride (8.5 g) and calcium carbonate (3.2 g) in methanol-water (9:1, 50 ml) and the mixture was stirred at reflux for 1 h. The reaction was filtered through hyflo, the filtrate was concentrated in vacuo and the resulting oil was dissolved in chloroform (50 ml). The resulting precipitate was removed by filtration, the solvent was evaporated and the residue was purified by FCC (System D 19:1→4:1) to give the title compound as a crystalline mass (1.4 g) m.p. 30°-31°.

후처리

  1. temperatureat reflux for 1 h
  2. filtrationThe reaction was filtered through hyflo
  3. concentrationthe filtrate was concentrated in vacuo
  4. dissolutionthe resulting oil was dissolved in chloroform (50 ml)
  5. customThe resulting precipitate was removed by filtration
  6. customthe solvent was evaporated
  7. customthe residue was purified by FCC (System D 19:1→4:1)

출처 및 근거

ORD 기록
ord-5f2ef6d99d184d2296edef7dfc469a1a
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853381

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