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Imidazole → HCID 14991429, 화합물

HRID 1196966
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HRID 1196966 반응식
N1C=CN=C1.[S:6]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C@@H:7]1[O:15][C@H:14]([CH2:16][OH:17])[C@@H:12]([OH:13])[C@H:10]([OH:11])[C@H:8]1[OH:9].[Si:24](Cl)([C:37]([CH3:40])([CH3:39])[CH3:38])([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.CO>CN(C=O)C.C(Cl)Cl.CCCCCC.CCOC(C)=O>[Si:24]([O:17][CH2:16][C@H:14]1[O:15][C@@H:7]([S:6][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[C@H:8]([OH:9])[C@@H:10]([OH:11])[C@@H:12]1[OH:13])([C:37]([CH3:40])([CH3:39])[CH3:38])([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
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참가 물질

9

반응물 4

HCID 795ImidazoleHCID 887Methanol2회HCID 94078tert-ButyldiphenylchlorosilaneHCID 10934592Phenyl 1-thio-beta-D-glucopyranoside

생성물 1

HCID 14991429HCID 14991429, 화합물수율 90.6%

시약·촉매·용매 4

HCID 6228
Dimethylformamide
용매
HCID 6344Dichloromethane용매
HCID 8058Hexane용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

Imidazole (32 g) is added to a solution of 3 (30 g) in DMF (225 mL). After cooling to 0° C., tert-butyldiphenylsilyl chloride (34 g) is added. The reaction is allowed to come to room temperature overnight, whereupon TLC analysis (silica, 10% MeOH in CH2Cl2) indicates that the reaction is complete. MeOH (30 mL) is added and the reaction is stirred for an additional 30 minutes. The solvents are then removed in vacuo (40° C., 10 mm Hg). The residue is dissolved in EtOAc (500 mL) and washed successively with water (2×100 mL) and brine (2×100 mL). The EtOAc solution is then dried (MgSO4) and filtered. Removal of the EtOAc in vacuo provides a syrup which is subjected to flash column chromatography (silica, 5% EtOAc in hexane) to provide phenyl 6-O-(tert-butyldiphenylsilyl)-1-thio-β-D-glucopyranoside (4, 51 g).

후처리

  1. customThe solvents are then removed in vacuo (40° C., 10 mm Hg)
  2. dissolutionThe residue is dissolved in EtOAc (500 mL)
  3. washwashed successively with water (2×100 mL) and brine (2×100 mL)
  4. dry with materialThe EtOAc solution is then dried (MgSO4)
  5. filtrationfiltered
  6. customRemoval of the EtOAc in vacuo
  7. customprovides a syrup which

출처 및 근거

ORD 기록
ord-5c24a39e12884ffb9eb27823fea68637
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05116821

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