Toluene → HCID 12939724, 화합물

HRID 1577466노트

반응식

HRID 1577466 반응식
C1(C)C=CC=CC=1.[CH3:8][C:9]([NH2:17])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[Cl:18][CH:19]([C:23]([CH3:26])([CH3:25])[CH3:24])[C:20](Cl)=[O:21]>N1C=CC=CC=1>[CH3:8][C:9]([NH:17][C:20](=[O:21])[CH:19]([C:23]([CH3:26])([CH3:25])[CH3:24])[Cl:18])([CH3:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 1140TolueneHCID 68509CumylamineHCID 12239723Butanoyl chloride, 2-chloro-3,3-dimethyl-

생성물 1

HCID 12939724HCID 12939724, 화합물수율 88.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Into a 200 ml four-necked flask, there were charged toluene (100 ml), α,α-dimethylbenzylamine (9 g) and pyridine (5.8 g), and α-chloro-tert-butylacetyl chloride (11.3 g) was dropwise added thereto while stirring at room temperature. Stirring was continued for 3 hours. The reaction mixture was washed with water to remove pyridine hydrochloride. After the toluene layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The obtained residue was recrystallized from ethanol to give 15.8 g of N-(α,α-dimethylbenzyl)-α-chloro-tert-butylacetamide. M.P., 159°-160° C.

후처리

  1. additionwas dropwise added
  2. stirringStirring
  3. washThe reaction mixture was washed with water
  4. customto remove pyridine hydrochloride
  5. dry with materialAfter the toluene layer was dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe obtained residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-8608a004a37241d7b420be51d9ac667e
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04288244

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