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Pyridine → Methyl 2,3,4-tri-O-benzyl-6-O-trifluoromethylsulfonyl-beta-D-glucopyranoside

HRID 2372162
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HRID 2372162 반응식
N1C=CC=CC=1.[F:7][C:8]([F:21])([F:20])[S:9]([O:12]S(C(F)(F)F)(=O)=O)(=[O:11])=[O:10].[CH2:22]([O:29][C@@H:30]1[C@@H:37]([O:38][CH2:39][C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)[C@H:36]([O:46][CH2:47][C:48]2[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=2)[C@@H:35]([CH2:54]O)[O:34][C@H:31]1[O:32][CH3:33])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>C(Cl)Cl>[CH2:22]([O:29][C@@H:30]1[C@@H:37]([O:38][CH2:39][C:40]2[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=2)[C@H:36]([O:46][CH2:47][C:48]2[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=2)[C@@H:35]([CH2:54][O:12][S:9]([C:8]([F:21])([F:20])[F:7])(=[O:11])=[O:10])[O:34][C@H:31]1[O:32][CH3:33])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 11113352methyl 2,3,4-tri-O-benzyl-beta-D-glucopyranoside

생성물 1

HCID 22842886Methyl 2,3,4-tri-O-benzyl-6-O-trifluoromethylsulfonyl-beta-D-glucopyranoside수율 89%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
-10 °C

실험 절차

To a solution of dry pyridine (0.456 mL) in methylene chloride (20 mL) cooled to -15° C. was added trifluoromethanesulfonic anhydride (0.864 mL). The mixture was stirred during 15 min at -10° C., then methyl 2,3,4-tri-O-benzyl-β-D-glucopyranoside (1.2 g, 2.58 mmol) in methylene chloride (30 mL) was added [P. Kovac, J. Alfoldi and M. Kosik, Chem. Zvesti 28, 820, (1974)]. The mixture was stirred during 1.5 h at -10° C. The reaction mixture was washed with water. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to afford an oil. Flash chromatography on silica gel and elution with a 7:2 mixture of hexane and ethyl acetate afforded the expected compound methyl 2,3,4-tri-O-benzyl-6-O-trifluoromethylsulfonyl -β-D-glucopyranoside (1.408 g, 89%) as an oil, which crystallized in the fridge.

후처리

  1. stirringThe mixture was stirred during 1.5 h at -10° C
  2. washThe reaction mixture was washed with water
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customto afford an oil
  7. washFlash chromatography on silica gel and elution
  8. additionwith a 7:2 mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-c8dd54ea4d554afeb5657d70f05e8a4b
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05097023

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