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Sodium Carbonate → HCID 67163472, 화합물

HRID 68624
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HRID 68624 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH2:14][C:15]1[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:25](=[O:28])([O-])[O-:26].[Na+].[Na+]>O.O1CCCC1.ClC(OCC1C=CC=CC=1)=O.C(OCC)(=O)C>[CH2:14]([O:26][C:25]([N:13]([CH2:14][C:15]1[CH:16]=[CH:17][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:23][CH:24]=1)[CH2:12][CH2:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7])=[O:28])[C:15]1[CH:24]=[CH:23][CH:18]=[CH:17][CH:16]=1
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참가 물질

7

반응물 2

HCID 10340Sodium CarbonateHCID 67163687HCID 67163687, 화합물

생성물 1

HCID 67163472HCID 67163472, 화합물수율 204.8%

시약·촉매·용매 4

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매
HCID 10387
Benzyl chloroformate
용매

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온도
0 °C

실험 절차

To a solution of the compound 3 (810 mg) and sodium carbonate (383 mg) in water (5 mL) and tetrahydrofuran (2 mL), benzyl chloroformate (413 μl) was added at 0° C. The reaction mixture was stirred at 0° C. for one hour. The reaction mixture was diluted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous sodium sulfate and then concentrated. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1→3:1) to obtain the title compound (1.16 g) having the following physical properties.

후처리

  1. washThe organic layer was washed with water and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1→3:1)

출처 및 근거

ORD 기록
ord-08aaded538ae4a78a1ac4d2d83cfc1d2
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822459B2

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