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Ethanol → HCID 14157593、化合物

HRID 1734238
ノート
印刷プレビュー

反応式

HRID 1734238 の反応式
[OH:1][CH2:2][C@@H:3]1[C@@H:7]([CH2:8][OH:9])[O:6][CH2:5][O:4]1.[C:10](OC(=O)C)(=[O:12])[CH3:11].[CH2:17]([OH:19])[CH3:18]>N1C=CC=CC=1>[C:10]([O:1][CH2:2][C@@H:3]1[C@@H:7]([CH2:8][O:9][C:17](=[O:19])[CH3:18])[O:6][CH2:5][O:4]1)(=[O:12])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 7918Acetic Anhydride2 回HCID 14157576(4R,5R)-4,5-bis(hydroxymethyl)-1,3-dioxolane

生成物 1

HCID 14157593HCID 14157593、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

The crude (4R,5R)-4,5-bis(hydroxymethyl)-1,3dioxolane obtained in Example 3 was dissolved in 300 ml of pyridine. After the addition of 150 g of excessive amount of acetic anhydride under ice cooling, the mixture was reacted for about 16 hours while stirring at room temperature. 20 ml of ethanol was added in portions while cooling over a water bath in order to decompose the excessive amount of acetic anhydride. After concentration by evaporator, the concentrate was extracted with 500 ml of ethyl acetate and washed with water, followed by removal of the solvent by evaporator. Although this product may be used for the next reaction as it was, the purification by silica gel column chromatography afforded 79.29 g of light yellow oil of (4R,5R)-4,5-bis(acetoxymethyl)-1,3-dioxolane.

後処理

  1. customthe mixture was reacted for about 16 hours
  2. temperaturewhile cooling over a water bath in order
  3. concentrationAfter concentration
  4. customby evaporator
  5. extractionthe concentrate was extracted with 500 ml of ethyl acetate
  6. washwashed with water
  7. customfollowed by removal of the solvent by evaporator
  8. customAlthough this product may be used for the next reaction as it
  9. customthe purification by silica gel column chromatography

出典と根拠

ORDレコード
ord-f78425838ddd476ab0034307ac7136b9
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05532380

反応ノート

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