Hydrochloric Acid → [5-(2-Ethoxyethoxy)-2-pyridyl]acetone

HRID 1086249노트

반응식

HRID 1086249 반응식
C([Li])CCC.[CH2:6]([O:8][CH2:9][CH2:10][O:11][C:12]1[CH:13]=[CH:14][C:15]([CH3:18])=[N:16][CH:17]=1)[CH3:7].CN(C)[C:21](=[O:23])[CH3:22].Cl>CCCCCC.O1CCCC1>[CH2:6]([O:8][CH2:9][CH2:10][O:11][C:12]1[CH:13]=[CH:14][C:15]([CH2:18][C:21](=[O:23])[CH3:22])=[N:16][CH:17]=1)[CH3:7]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 31374DimethylacetamideHCID 150671045-(2-Ethoxyethoxy)-2-methylpyridineHCID 178418339Butyllithium

생성물 1

HCID 15067111[5-(2-Ethoxyethoxy)-2-pyridyl]acetone

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매3회HCID 8058Hexane용매

실험 절차

2.5 ml of a 2.5 M solution of n-butyllithium in hexane are added dropwise at 5° C. to a solution of 1 g (5.5 mmol) of 5-(2-ethoxyethoxy)-2-methylpyridine in 20 ml of tetrahydrofuran. The mixture is stirred at 0°-5° C. for 10 minutes and then 530 mg (6 mmol) of N,N-dimethylacetamide dissolved in a little tetrahydrofuran are added. After stirring at room temperature for 90 minutes, the pH is adjusted to 5 with dilute hydrochloric acid and the tetrahydrofuran is stripped off. The residue is extracted with ethyl acetate, and the organic phase is dried with sodium sulphate and evaporated. Yield: 580 mg (47% of theory), content according to GC/MS: 75%.

후처리

  1. additionare added
  2. stirringAfter stirring at room temperature for 90 minutes
  3. extractionThe residue is extracted with ethyl acetate
  4. dry with materialthe organic phase is dried with sodium sulphate
  5. customevaporated

출처 및 근거

ORD 기록
ord-c33e8bb245504f4dae515bdc12f81a24
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05028617

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