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Potassium Bicarbonate → HCID 67348403, 화합물

HRID 910591
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HRID 910591 반응식
C([N:4]1[C:8]([CH3:9])=[C:7]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:6]([O:17][C@@H:18]2[O:44][C@H:43]([CH2:45][O:46][C:47](=[O:52])[C:48]([CH3:51])([CH3:50])[CH3:49])[C@@H:35]([O:36][C:37](=[O:42])[C:38]([CH3:41])([CH3:40])[CH3:39])[C@H:27]([O:28][C:29](=[O:34])[C:30]([CH3:33])([CH3:32])[CH3:31])[C@H:19]2[O:20][C:21](=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23])=[N:5]1)(=O)C.C(=O)(O)[O-].[K+]>CO>[CH2:10]([C:7]1[C:6]([O:17][C@@H:18]2[O:44][C@H:43]([CH2:45][O:46][C:47](=[O:52])[C:48]([CH3:51])([CH3:50])[CH3:49])[C@@H:35]([O:36][C:37](=[O:42])[C:38]([CH3:39])([CH3:40])[CH3:41])[C@H:27]([O:28][C:29](=[O:34])[C:30]([CH3:33])([CH3:32])[CH3:31])[C@H:19]2[O:20][C:21](=[O:26])[C:22]([CH3:23])([CH3:24])[CH3:25])=[N:5][NH:4][C:8]=1[CH3:9])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 516893Potassium BicarbonateHCID 67350156HCID 67350156, 화합물

생성물 1

HCID 67348403HCID 67348403, 화합물수율 95.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 1-acetyl-4-benzyl-5-methyl-3-(2,3,4,6-tetra-O-pivaloyl-β-D-glucopyranosyloxy)-1H-pyrazole (1.00 g) in methanol (10 mL) was added potassium bicarbonate (0.058 g) under stirring at room temperature. The reaction mixture was stirred at room temperature for 16 hours. After the precipitation of the crystals by the addition of a solution of glacial acetic acid (0.034 g) in water (20 mL) at room temperature, the mixture was stirred for 2 hours. After the suspension was stirred under ice-cooling for 1 hour, the crystals were collected by filtration. The obtained crystals were washed with a mixed solution of 2-propanol and n-heptane, and dried under reduced pressure to give 4-benzyl-5-methyl-3-(2,3,4,6-tetra-O-pivaloyl-β-D-glucopyranosyloxy)-1H-pyrazole (0.90 g).

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 16 hours
  2. customAfter the precipitation of the crystals
  3. additionby the addition of a solution of glacial acetic acid (0.034 g) in water (20 mL) at room temperature
  4. stirringthe mixture was stirred for 2 hours
  5. stirringAfter the suspension was stirred under ice-
  6. temperaturecooling for 1 hour
  7. filtrationthe crystals were collected by filtration
  8. washThe obtained crystals were washed with a mixed solution of 2-propanol and n-heptane
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-9bcace9b8bb64049b9a21d1231133aec
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022192B2

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