Hydrochloric Acid → HCID 10261437、化合物

HRID 2116668ノート

反応式

HRID 2116668 の反応式
[CH3:1][CH:2]([C:5]#[N:6])[C:3]#[N:4].Br[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].C(=O)([O-])[O-].[K+].[K+].Cl>CS(C)=O>[CH2:12]([O:11][C:9]([CH2:8][C:2]([CH3:1])([C:5]#[N:6])[C:3]#[N:4])=[O:10])[CH3:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 194252-Methylpropanedinitrile

生成物 1

HCID 10261437HCID 10261437、化合物収率 24.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

2.0 g of 2-methylmalononitrile and 4.2 g of ethyl bromoacetate were dissolved in 10 ml of dimethyl sulfoxide. 3.4 g of potassium carbonate was added thereto and stirred for 4 hours at room temperature. Then, to the reaction mixture was added dilute hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was subjected to silica gel column chromatography to give 1.0 g of 2-(ethoxycarbonylmethyl)-2-methylmalononitrile (hereinafter referred to as the present invention compound (74)).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed successively with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue obtained

出典と根拠

ORDレコード
ord-6bfe6cba5082434ea2e3f139004d1f58
出典データセット
uspto-grants-2008_10
特許番号
US07439266B2

反応ノート

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