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3,4-dihydro-2H-pyran → HCID 21714364, 화합물

HRID 355698
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HRID 355698 반응식
[CH3:1][N:2]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][C:7]=1[N+:16]([O-:18])=[O:17])[CH2:3][CH2:4][OH:5].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[O:31]1[CH:36]=[CH:35][CH2:34][CH2:33][CH2:32]1.C(=O)([O-])O.[Na+]>O1CCCC1>[CH3:1][N:2]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][C:7]=1[N+:16]([O-:18])=[O:17])[CH2:3][CH2:4][O:5][CH:32]1[CH2:33][CH2:34][CH2:35][CH2:36][O:31]1
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참가 물질

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HCID 80803,4-dihydro-2H-pyranHCID 516892Sodium BicarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 27795662-{Methyl[2-nitro-4-(trifluoromethyl)phenyl]amino}ethan-1-ol

생성물 1

HCID 21714364HCID 21714364, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

A mixture of 4-[N-methyl--N-(2-hydroxyethyl)-amino]-3-nitrobenzotrifluoride (29.0 g, 110 mmol), p-toluenesulfonic acid monohydrate (2.09 g, 11.0 mmol), 3,4-dihydro-2H-pyran (18.5 g, 220 mmol) and tetrahydrofuran (600 ml) was stirred at room temperature for 4.5 hours. Sodium hydrogencarbonate (10 g) was added to the reaction mixture and the resulting mixture was stirred at room temperature for 30 minutes, after which the insoluble materials were filtered off. The filtrate was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: ethyl acetate/n-hexane= 5/95) to obtain an oil of 4-[N-methyl-N-[2-(2-tetrahydro-2H-pyranyl) oxyethyl]amino]-3-nitrobenzotrifluoride.

후처리

  1. stirringthe resulting mixture was stirred at room temperature for 30 minutes
  2. filtrationafter which the insoluble materials were filtered off
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe resulting residue was purified by a silica gel column chromatography (eluent: ethyl acetate/n-hexane= 5/95)

출처 및 근거

ORD 기록
ord-2bf21cc5013c42a69c3939e3f260cb48
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05834454

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