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Potassium Carbonate → HCID 58504138, 화합물

HRID 2407787
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HRID 2407787 반응식
[CH3:1][O:2][CH:3]([O:40][CH3:41])[CH2:4][N:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18](=[O:39])[CH2:19][CH2:20][CH:21]1[CH2:26][CH2:25][N:24]([CH2:27][C:28]2[S:32][C:31]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=3)=[N:30][CH:29]=2)[CH2:23][CH2:22]1)[C:6](=O)[C:7]([O:9][CH3:10])=[O:8].C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:1][O:2][CH:3]([O:40][CH3:41])[CH2:4][N:5]1[C:12]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:18](=[O:39])[C:19]([CH2:20][CH:21]2[CH2:22][CH2:23][N:24]([CH2:27][C:28]3[S:32][C:31]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=4)=[N:30][CH:29]=3)[CH2:25][CH2:26]2)=[C:6]1[C:7]([O:9][CH3:10])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 58504269HCID 58504269, 화합물

생성물 1

HCID 58504138HCID 58504138, 화합물수율 90%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The compound prepared in Example 324 (0.390 g) was suspended in methanol (7 mL) and potassium carbonate (0.093 g) added. The reaction mixture was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure to afford the crude material, which was partitioned between ethyl acetate and water. The organics were washed with brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure to afford the crude product, which was purified by flash column chromatography (eluant: 5% (9:1 methanol/concentrated ammonium hydroxide)/ethyl acetate) to furnish the title compound (0.340 g) having the following physical properties.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto afford the crude material, which
  3. customwas partitioned between ethyl acetate and water
  4. washThe organics were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customto afford the crude product, which
  9. customwas purified by flash column chromatography (eluant: 5% (9:1 methanol/concentrated ammonium hydroxide)/ethyl acetate)

출처 및 근거

ORD 기록
ord-49ef056f675b4fb997e8a8f4bbb545c0
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809538B2

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