Diethyl Ether → 2,2-Dichloro-3-oxocyclobutyl pivalate

HRID 473368

反応式

HRID 473368 の反応式
[C:1](OC=C)(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].Cl[C:11]([Cl:16])([Cl:15])[C:12](Cl)=[O:13].[O-][Mn](=O)(=O)=O.[K+].[CH3:23][CH2:24][O:25]CC>[Zn]>[C:1]([O:13][CH:12]1[CH2:23][C:24](=[O:25])[C:11]1([Cl:16])[Cl:15])(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3]

参加物

6

反応物 4

HCID 3283Diethyl Ether2 回HCID 6420Trichloroacetyl chlorideHCID 256591Vinyl pivalateHCID 516875Potassium Permanganate

生成物 1

HCID 575158702,2-Dichloro-3-oxocyclobutyl pivalate

試薬・触媒・溶媒 1

HCID 23994Zinc触媒

反応条件

温度
22.5 °C

実験手順

To a stirred mixture of vinyl pivalate (30 g, 234 mmol) and zinc (31 g, 468 mmol) in ether (300 ml) was added a solution of 2,2,2-trichloroacetyl chloride (55 g, 304 mmol) in ether (300 ml) dropwise (2-3 h) in a water bath. (Note: fast addition causes the reaction temp. to elevate) while maintaining the reaction temperature between 15-30° C. After the reaction was done (stained with KMnO4 solution), it was filtered through Celite. The filtrate was washed with cold water, brine, dried over MgSO4 and concentrated to give the title compound as an orange solid.

後処理

  1. addition(Note: fast addition
  2. customthe reaction temp
  3. filtrationwas filtered through Celite
  4. washThe filtrate was washed with cold water, brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-052960677a784869b91cdc966dd857ae
出典データセット
uspto-grants-2014_01
特許番号
US08633315B2

関連ノート

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