Hydrochloric Acid → 2-(4-Chlorophenyl)-2-methylpropanal

HRID 610845ノート

反応式

HRID 610845 の反応式
[H-].C([Al+]CC(C)C)C(C)C.[Cl:11][C:12]1[CH:22]=[CH:21][C:15]([C:16]([CH3:20])([CH3:19])[C:17]#N)=[CH:14][CH:13]=1.[OH2:23].Cl>CCCCCC.C(OCC)C>[Cl:11][C:12]1[CH:22]=[CH:21][C:15]([C:16]([CH3:20])([CH3:19])[CH:17]=[O:23])=[CH:14][CH:13]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 101302194-Chloro-α,α-dimethylbenzeneacetonitrileHCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 114353342-(4-Chlorophenyl)-2-methylpropanal収率 94%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒

実験手順

Diisobutylaluminum hydride (0.236 mol, 236 mL of a 1M solution in hexane) is added over 90 minutes to a solution of p-chloro-α-methylhydratroponitrile (32.6 g, 0.181 mol) in diethyl ether under nitrogen at 0° C. After the addition is complete, water and 6N hydrochloric acid are added to the reaction mixture while maintaining the temperature below 30° C. The resultant aqueous solution is stirred overnight at room temperature and extracted with diethyl ether The organic extracts are combined, washed sequentially with 2N hydrochloric acid and water, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title product as an oil (31.1 g, 94% yield).

後処理

  1. additionAfter the addition
  2. temperaturewhile maintaining the temperature below 30° C
  3. extractionextracted with diethyl ether The organic extracts
  4. washwashed sequentially with 2N hydrochloric acid and water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2550eb0f5fe74f7397ad3bb2d8d74d35
出典データセット
uspto-grants-1999_12
特許番号
US05998673

反応ノート

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