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

HRID 877942ノート

反応式

HRID 877942 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 74236Tetrabutylammonium Bromide触媒

反応条件

温度
27.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-39710b81b78c4c13afa29ee5dc0b9e9e
出典データセット
uspto-grants-2015_03
特許番号
US08987444B2

反応ノート

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