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

HRID 1458383노트

반응식

HRID 1458383 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 114353342-(4-Chlorophenyl)-2-methylpropanal수율 94%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8058Hexane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-c922d7c151084ddfaf47b874f93c2219
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849958

반응 노트

불러오는 중…