Sulfuric Acid → N-[1,1-dimethyl-2-(2,4,6-trimethylphenyl)ethyl]formamide

HRID 966102ノート

反応式

HRID 966102 の反応式
[C-]#[N:2].[K+].S(=O)(=O)(O)O.[CH3:9][C:10](O)([CH3:21])[CH2:11][C:12]1[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=1[CH3:20].[C:23](=[O:26])([O-])[O-].[Na+].[Na+]>C(O)(=O)C>[CH3:9][C:10]([NH:2][CH:23]=[O:26])([CH3:21])[CH2:11][C:12]1[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=1[CH3:20]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 9032Potassium CyanideHCID 10340Sodium CarbonateHCID 223145482-Methyl-1-(2,4,6-trimethylphenyl)propan-2-ol

生成物 1

HCID 22314552N-[1,1-dimethyl-2-(2,4,6-trimethylphenyl)ethyl]formamide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

90 mL of glacial acetic acid and 33 g of potassium cyanide are combined while cooling with ice. 90 mL of sulfuric acid and 90 mL of glacial acetic acid are then added dropwise at 20° C. 65 g of 2-methyl-1-(2,4,6-trimethylphenyl)propan-2-ol is slowly added to the solution at constant temperature. After the addition has ended, the mixture is stirred for a further hour. The mixture is poured onto ice water, neutralized with sodium carbonate solution, and extracted with diethyl ether. The solvent is distilled off under reduced pressure and the residue is fractionally distilled. Yield: 55 g (74%); bp0.1: 155° C.

後処理

  1. temperaturewhile cooling with ice
  2. additionAfter the addition
  3. additionThe mixture is poured onto ice water
  4. extractionextracted with diethyl ether
  5. distillationThe solvent is distilled off under reduced pressure
  6. distillationthe residue is fractionally distilled
  7. custom155° C.

出典と根拠

ORDレコード
ord-68ba0bacb06145f1b0b9d0110ba4a991
出典データセット
uspto-grants-2005_10
特許番号
US06951888B2

反応ノート

読み込み中…