Sodium → HCID 13770583, 화합물

HRID 236227노트

반응식

HRID 236227 반응식
[Na].Cl[CH2:3][CH2:4][CH:5]([CH3:20])[C:6]([NH:8][C:9]1[S:10][CH:11]=[C:12]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:13]=1[C:14]#[N:15])=[O:7]>C(O)C>[C:14]([C:13]1[C:12]([C:16]([CH3:19])([CH3:18])[CH3:17])=[CH:11][S:10][C:9]=1[N:8]1[CH2:3][CH2:4][CH:5]([CH3:20])[C:6]1=[O:7])#[N:15]

참가 물질

4

반응물 2

HCID 5360545SodiumHCID 13770589HCID 13770589, 화합물

생성물 1

HCID 13770583HCID 13770583, 화합물수율 75%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To a solution of 0.21 g of sodium dissolved in 10 ml of ethanol was added 2.75 g of 4-chloro-N-[3-cyano-4-(1,1-dimethylethyl)-2-thienyl]-2-methylbutanamide dissolved in 35 ml ethanol dropwise. The mixture was allowed to stir at room temperature for about one hour and the solvent was removed in vacuo. The residue was combined with 10 ml ethanol and 250 ml water and the precipitate was collected by filtration. The collected solid was recrystallized from hexane to afford 1.8 g of N-[3-cyano-4-(1,1-dimethylethyl)-2-thienyl]-3-methyl-2-pyrrolidinone. Yield 75%. mp=92°-94° C.

후처리

  1. customthe solvent was removed in vacuo
  2. filtrationthe precipitate was collected by filtration
  3. customThe collected solid was recrystallized from hexane

출처 및 근거

ORD 기록
ord-df30eafc0ee543eb824b4181757cfbd0
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04643758

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