Sodium Acetate → ethyl 2-((4R,6S)-6-(acetoxymethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate

HRID 877942노트

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HRID 877942 반응식
Cl[CH2:2][C@H:3]1[O:8][C:7]([CH3:10])([CH3:9])[O:6][C@@H:5]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:4]1.[C:17]([O-:20])(=[O:19])[CH3:18].[Na+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[C:17]([O:20][CH2:2][C@H:3]1[O:8][C:7]([CH3:10])([CH3:9])[O:6][C@@H:5]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:4]1)(=[O:19])[CH3:18]

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 67323517ethyl 2-((4R,6S)-6-(chloromethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate

생성물 1

HCID 53339171ethyl 2-((4R,6S)-6-(acetoxymethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate

시약·촉매·용매 1

HCID 74236Tetrabutylammonium Bromide촉매

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온도
27.5 °C

실험 절차

Mixture of ethyl 2-((4R,6S)-6-(chloromethyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate (60 grams), tetra butyl ammonium bromide (79 grams) and anhydrous sodium acetate (61.2 grams) was heated to reflux temperature and stirred. After the completion of the reaction, the reaction mixture was cooled to 25-30° C. and petroleum ether (50 ml) was added to it then stirred for 60 minutes at 25-30° C. The reaction mixture was filtered and washed with petroleum ether. The solvent from the filtrate was distilled off under reduced pressure to get the title compound.

후처리

  1. temperaturewas heated
  2. temperatureto reflux temperature
  3. customAfter the completion of the reaction
  4. stirringthen stirred for 60 minutes at 25-30° C
  5. filtrationThe reaction mixture was filtered
  6. washwashed with petroleum ether
  7. distillationThe solvent from the filtrate was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-39710b81b78c4c13afa29ee5dc0b9e9e
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987444B2

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