Triethylamine → HCID 131723194, 화합물

HRID 843211노트

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HRID 843211 반응식
[CH3:1][C@@H:2]([OH:12])[C@@H:3]([OH:11])[C@H:4]([O:9][CH3:10])[C@@H:5]([OH:8])[CH:6]=[O:7].[CH3:13][C@H:14]1[O:19][C@@H:18]([OH:20])[CH2:17][C@H:16]([O:21][CH3:22])[C@@H:15]1[OH:23].[Sn](Cl)Cl.C(N(CC)CC)C>ClCCl.FC(F)(F)S([O-])(=O)=O.[Ag+]>[CH3:1][C@@H:2]([OH:12])[C@@H:3]([OH:11])[C@H:4]([O:9][CH3:10])[C@@H:5]([OH:8])[CH:6]=[O:7].[CH3:13][C@H:14]1[O:19][C@@H:18]([OH:20])[CH2:17][C@H:16]([O:21][CH3:22])[C@@H:15]1[OH:23]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 24479Stannous ChlorideHCID 193394AcofrioseHCID 4414172,6-Dideoxy-3-O-methylhexopyranose

생성물 1

HCID 131723194HCID 131723194, 화합물수율 15%

시약·촉매·용매 2

HCID 76223Silver(I) trifluoromethanesulfonate촉매HCID 6344Dichloromethane용매

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온도
-15 °C

실험 절차

A solution of thevetose (50 A) (1,5 g), cymarose (40) (1,3 g), and molecular sieves 4 Å in dichloromethane is stirred at room temperature for 1 hour. The reaction mixture is cooled to −15° C., and tin (II) chloride (0,8 g) and silver trifluoromethanesulphonate (1,1 g) are added. The mixture is stirred at −15° C. for 16 hours, after which triethylamine (0,5 ml) is added. The reaction product is filtered and the dichloromethane is evaporated. The dissaccharide (53) is purified by silica gel column chromatography eluting with ethyl acetate:hexane (2:8), yield 15%.

후처리

  1. filtrationThe reaction product is filtered
  2. customthe dichloromethane is evaporated
  3. customThe dissaccharide (53) is purified by silica gel column chromatography
  4. washeluting with ethyl acetate:hexane (2:8), yield 15%

출처 및 근거

ORD 기록
ord-60f0ea786d13431096096d5ab4ac2b4c
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06376657B1

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