Methanol → HCID 15521806、化合物

HRID 356809

反応式

HRID 356809 の反応式
O[CH:2]([OH:6])[C:3](=[O:5])[CH3:4].N1[CH:12]=[CH:11][CH:10]=CC=1.[C:13]([O:18]C(=O)C(C)C)(=[O:17])[CH:14]([CH3:16])[CH3:15].[CH3:24][OH:25]>CN(C)C1C=CN=CC=1.C(OCC)(=O)C>[C:13]([O:18][CH2:4][C:3]([CH2:2][O:6][C:24](=[O:25])[CH:11]([CH3:10])[CH3:12])=[O:5])(=[O:17])[CH:14]([CH3:16])[CH3:15]

参加物

7

反応物 4

HCID 887MethanolHCID 1049PyridineHCID 7346Isobutyric anhydrideHCID 131809821,1-Dihydroxypropan-2-one

生成物 1

HCID 15521806HCID 15521806、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8857Ethyl Acetate溶媒

実験手順

A 100 ml reaction vessel was charged with 4.18 g of dihydroxyacetone (monomer), 11.2 ml of pyridine and 10 mg of 4-dimethylaminopyridine and the mixture was stirred at room temperature. Thereto was added dropwise 16.7 ml of isobutyric anhydride over 30 minutes. After the dropping, the resulting liquid was further stirred for 1 hour and then 1 ml of methanol was added thereto and the resulting liquid was further stirred for 1 hour. To the reaction mixture was added ethyl acetate and the organic layer was separated. The organic layer was washed with water and further washed with saturated aqueous solution with sodium bicarbonate and 1N HCl. Then, the solvent was removed under reduced pressure. The residue was distilled under reduced pressure to give 7.47 g of the desired compound.

後処理

  1. customA 100 ml reaction vessel
  2. stirringAfter the dropping, the resulting liquid was further stirred for 1 hour
  3. stirringthe resulting liquid was further stirred for 1 hour
  4. customthe organic layer was separated
  5. washThe organic layer was washed with water
  6. washfurther washed with saturated aqueous solution with sodium bicarbonate and 1N HCl
  7. customThen, the solvent was removed under reduced pressure
  8. distillationThe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-a997e571454d4d2ca8243fa3c1bb3cc0
出典データセット
uspto-grants-1998_11
特許番号
US05840553

関連ノート

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