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Methanesulfonic Acid → HCID 68015078, 화합물

HRID 1913025
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HRID 1913025 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]([Cl:18])=[C:6]([CH2:8][C:9]2[CH:10]=[CH:11][C:12]3[O:16][CH2:15][CH2:14][C:13]=3[CH:17]=2)[CH:7]=1.[Li][CH2:20]CCC.CCCCCC.C[Si](C)(C)[O:32][C@@H:33]1[C@@H:38]([O:39][Si](C)(C)C)[C@H:37]([O:44][Si](C)(C)C)[C@@H:36]([CH2:49][O:50][Si](C)(C)C)[O:35][C:34]1=[O:55].CS(O)(=O)=O>C1(C)C=CC=CC=1.CO>[Cl:18][C:5]1[CH:4]=[CH:3][C:2]([C@@:34]2([O:55][CH3:20])[C@H:33]([OH:32])[C@@H:38]([OH:39])[C@H:37]([OH:44])[C@@H:36]([CH2:49][OH:50])[O:35]2)=[CH:7][C:6]=1[CH2:8][C:9]1[CH:10]=[CH:11][C:12]2[O:16][CH2:15][CH2:14][C:13]=2[CH:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 6395Methanesulfonic AcidHCID 8058HexaneHCID 10994280(3R,4S,5R,6R)-3,4,5-Tris-trimethylsilanyloxy-6-trimethylsilanyloxymethyl-tetrahydro-pyran-2-onHCID 68015074HCID 68015074, 화합물HCID 178418339Butyllithium

생성물 1

HCID 68015078HCID 68015078, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매

반응 조건

온도
-78 °C

실험 절차

5-[(5-bromo-2-chloro-phenyl)methyl]-2,3-dihydrobenzofuran 5d (10.0 g, 30.9 mmol) was dissolved in 90 mL of mixed solution (THF and toluene, v:v=1:2) and cooled to −78° C., followed by dropwise addition of a solution of nBuLi in n-hexane (14.83 mL, 37.1 mmol). After stirring for 1 hour at −78° C., a solution of (3R,4S,5R,6R)-3,4,5-tris(trimethylsilyloxy)-6-(trimethylsilyloxymethyl)tetrahydropyran-2-one 2f (15.87 g, 33.9 mmol) in toluene (90 mL) was dropwise added before the reaction mixture was stirred for 3 hours at −78° C. A solution of 0.6 M methanesulfonic acid in methanol (103 mL) was added before the reaction mixture was stirred for 16 hours. Thereafter, the reaction was concentrated under reduced pressure after 100 mL saturated sodium carbonate solution were added. The residue was extracted with ethyl acetate (100 mL×3) after 50 mL saturated sodium chloride solution were added and the organic extract was combined, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system E to obtain the title compound (2S,3R,4S,5S,6R)-2-[4-chloro-3-(2,3-dihydrobenzofuran-5-ylmethyl)phenyl]-6-(hydroxymethyl)-2-methoxy-tetrahydropyran-3,4,5-triol 5e (6.3 g, white solid), yield: 46.7%. 1H NMR (400 MHz, CD3OD): δ 7.53 (d, 1H), 7.45 (dd, 1H), 7.35 (d, 1H), 7.03 (s, 1H), 6.91 (d, 1H), 6.60 (d, 1H), 4.48 (t, 2H), 4.13-3.91 (m, 3H), 3.84-3.73 (m, 2H), 3.61-3.56 (m, 1H), 3.44-3.39 (m, 1H), 3.11 (dd, 3H), 3.07 (s, 3H).

후처리

  1. stirringwas stirred for 3 hours at −78° C
  2. stirringwas stirred for 16 hours
  3. concentrationThereafter, the reaction was concentrated under reduced pressure after 100 mL saturated sodium carbonate solution
  4. additionwere added
  5. extractionThe residue was extracted with ethyl acetate (100 mL×3) after 50 mL saturated sodium chloride solution
  6. additionwere added
  7. extractionthe organic extract
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. concentrationThe filtrate was concentrated under reduced pressure
  11. customthe resulting residue was purified by silica gel chromatography with elution system E

출처 및 근거

ORD 기록
ord-fe8e3ac51a9b44fe8ef63ca89e897dd7
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08609622B2

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