Hydrogen Peroxide → HCID 44236488、化合物

HRID 1500248ノート

反応式

HRID 1500248 の反応式
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][C:7]([CH3:12])([CH3:11])[CH2:8][C:9]#[N:10])=[CH:4][CH:3]=1.OO.C(=O)([O-])[O-:18].[K+].[K+].O>CS(C)=O.C(Cl)Cl>[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][C:7]([CH3:11])([CH3:12])[CH2:8][C:9]([NH2:10])=[O:18])=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 962WaterHCID 11430Potassium CarbonateHCID 58155372HCID 58155372、化合物

生成物 1

HCID 44236488HCID 44236488、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-(4-chlorophenoxy)-3-methylbutyronitrile (60.4 mmol) in DMSO (75 mL) is treated with H2O2 (50% w/w) (434 mmol) and potassium carbonate (121 mmol) at zero degrees Celsius. The reaction mixture is stirred at room temperature over the weekend. The reaction mixture is transferred into a separatory funnel using water (100 mL) and CH2Cl2 (200 mL). The mixture is equilibrated and the CH2Cl2 layer is removed. The aqueous layer is extracted two additional times with CH2Cl2 (2×300 mL). The combined CH2Cl2 extracts are washed 5 consecutive times with water (5×200 mL) followed by a brine (500 mL) wash, dried over anhydrous MgSO4, filtered, and concentrated under reduced pressure, which affords 3-(4-chlorophenoxy)-3-methylbutyramide.

後処理

  1. customThe reaction mixture is transferred into a separatory funnel
  2. customthe CH2Cl2 layer is removed
  3. extractionThe aqueous layer is extracted two additional times with CH2Cl2 (2×300 mL)
  4. washThe combined CH2Cl2 extracts are washed 5 consecutive times with water (5×200 mL)
  5. washwash
  6. dry with materialdried over anhydrous MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure, which

出典と根拠

ORDレコード
ord-8b3384ac7b09499d8b17aa0c6fc716ae
出典データセット
uspto-grants-2015_12
特許番号
US09206143B2

反応ノート

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