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HCID 11096141、化合物 → HCID 86601630、化合物

HRID 1268710
ノート
印刷プレビュー

反応式

HRID 1268710 の反応式
[CH3:1][C:2]1([CH3:14])[O:6][C@H:5]2[CH2:7][S:8][C@H:9]([C@H:10]([OH:13])CO)[C@H:4]2[O:3]1>C(OCC)(=O)C.C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Pb+4]>[CH3:1][C:2]1([CH3:14])[O:6][C@H:5]2[CH2:7][S:8][C@H:9]([CH:10]=[O:13])[C@H:4]2[O:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 11096141HCID 11096141、化合物

生成物 1

HCID 86601630HCID 86601630、化合物収率 99.6%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 178418268HCID 178418268、化合物溶媒

実験手順

2.5 g (11.2 mmol) of (1R)-1-((3aS,4R,6aR)-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxol-4-yl)-ethane-1,2-diol from the aforementioned Experimental Example 5 were dissolved in ethyl acetate to which lead tetraacetate were added at 0° C., and the reaction mixture was stirred for 10 min. The reaction mixture was filtered. Ethyl acetate was added to the filtrate, which was washed with saturated sodium bicarbonate, dried, and filtered. The filtrate was concentrated under reduced pressure, and the concentrate was purified by silica gel column chromatography using the eluant (hexane:ethyl acetate=5:1) to obtain 2.1 g (yield: 98%) of (3aS,4S,6aR)-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxole-4–Carbaldehyde as an oil.

後処理

  1. additionwere added at 0° C.
  2. filtrationThe reaction mixture was filtered
  3. additionEthyl acetate was added to the filtrate, which
  4. washwas washed with saturated sodium bicarbonate
  5. customdried
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe concentrate was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-5104219b74d34fef96b7f51a3c42687c
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07199127B2

反応ノート

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