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Methanesulfonic Acid → HCID 68015078、化合物

HRID 1913025
ノート
印刷プレビュー

反応式

HRID 1913025 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

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

生成物 1

HCID 68015078HCID 68015078、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1140Toluene溶媒

反応条件

温度
-78 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fe8e3ac51a9b44fe8ef63ca89e897dd7
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609622B2

反応ノート

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