Methanol → HCID 15521806, 화합물

HRID 356809

반응식

HRID 356809 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

HCID 15521806HCID 15521806, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a997e571454d4d2ca8243fa3c1bb3cc0
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840553

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