HCID 67809616、化合物 → HCID 19389468、化合物

HRID 1757046ノート

反応式

HRID 1757046 の反応式
[Si:1]([O:8][CH2:9][CH:10]1[O:15][C:14](=[O:16])[CH:13]=[C:12]([OH:17])[CH2:11]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]>C(O)C>[Si:1]([O:8][CH2:9][CH:10]1[O:15][C:14](=[O:16])[CH2:13][CH:12]([OH:17])[CH2:11]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

参加物

3

反応物 1

HCID 67809616HCID 67809616、化合物

生成物 1

HCID 19389468HCID 19389468、化合物収率 96%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

6-t-Butyldimethylsilyloxymethyl-5,6-dihydro-4-hydroxy pyran-2-one (26.3 parts) was dissolved in ethanol (500 parts) and heated to 45° C.-55° C. Raney nickel (6.6 parts) was washed caustic free with water and then water free with ethanol and added to the pyran-2-one solution under a blanket of nitrogen. Hydrogen was passed through the rapidly stirred mixture until the reaction was complete, as judged by GC analysis. The catalyst was filtered off and the solvent removed at 40° C./20 mm to leave 6-t-butyldimethylsilyloxymethyl-4-hydroxytetrahydro pyran-2-one (25.7 parts, 96%, cis/trans ratio 82/18) as a greenish oil which solidified on standing.

後処理

  1. temperatureheated to 45° C.-55° C
  2. washRaney nickel (6.6 parts) was washed caustic free with water
  3. additionwater free with ethanol and added to the pyran-2-one solution under a blanket of nitrogen
  4. filtrationThe catalyst was filtered off
  5. customthe solvent removed at 40° C./20 mm

出典と根拠

ORDレコード
ord-10fca33d8a424f7f8797511275ff703f
出典データセット
uspto-grants-1995_08
特許番号
US05443970

反応ノート

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