Phosphoric Acid → (4R)-2,2-Dimethyl-1,3-dioxolane-4-carboxylic acid

HRID 41823ノート

反応式

HRID 41823 の反応式
[CH3:1][C:2]1([CH3:10])[O:6][C@@H:5]([C:7]([O-:9])=[O:8])[CH2:4][O:3]1.[Na+].OP(O)(O)=O.[Na+].[Cl-]>O.C(OCC)(=O)C>[CH3:1][C:2]1([CH3:10])[O:6][C@@H:5]([C:7]([OH:9])=[O:8])[CH2:4][O:3]1

参加物

6

反応物 3

HCID 1004Phosphoric AcidHCID 5234Sodium ChlorideHCID 23717304Sodium (R)-2,2-dimethyl-1,3-dioxolane-4-carboxylate

生成物 1

HCID 10855606(4R)-2,2-Dimethyl-1,3-dioxolane-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

Sodium (R)-(+)-2,2-dimethyl-1,3-dioxolane-4-carboxylate (1.03 g, 6.1 mmol) was dissolved in a mixture of water (1.2 ml) and ethyl acetate (1.2 ml) and cooled to 0° C. 2 M aqueous H3PO4 solution (7 ml) was added until the reaction mixture reached pH 2. After that the reaction mixture was saturated with NaCl and the reaction mixture was extracted with ethyl acetate (3×20 ml). The organic layer was dried over Na2SO4 and the solvent was removed under reduced pressure. The product (0.73 g, 4.9 mmol, 81%) was used in the next step without any further purification.

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate (3×20 ml)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-d9ce012cb251460a80633ea02b008e4b
出典データセット
uspto-grants-2013_09
特許番号
US08535655B2

反応ノート

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