Ethyl Acetate → Ethyl 4-cyano-4-(3-cyano-5-thienyl)-5-methylhexanate

HRID 1071624노트

반응식

HRID 1071624 반응식
[CH3:1]C(C)([O-])C.[K+].[C:7]([C:9]1[CH:13]=[C:12]([CH:14]([C:18]#[N:19])[CH:15]([CH3:17])[CH3:16])[S:11][CH:10]=1)#[N:8].[C:20]([O:23][CH2:24][CH3:25])(=[O:22])[CH3:21]>CN(C=O)C>[C:18]([C:14]([C:12]1[S:11][CH:10]=[C:9]([C:7]#[N:8])[CH:13]=1)([CH:15]([CH3:16])[CH3:17])[CH2:1][CH2:21][C:20]([O:23][CH2:24][CH3:25])=[O:22])#[N:19]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 223936703-Cyano-5-(1-cyano-2-methylpropyl]thiopheneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 22393597Ethyl 4-cyano-4-(3-cyano-5-thienyl)-5-methylhexanate수율 60%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

Potassium tert-butoxide (35 mg) was suspended in DMF (5 ml), and a DMF solution (5 ml) of 3-cyano-5-(1-cyano-2-methylpropyl]thiophene (0.60 g) was added thereto. After stirring at room temperature for 3.5 hours, ethyl acetate was added. The mixture was washed with an aqueous saturated ammonium chloride and further brine, dried over anhydrous magnesium sulfate and then evaporated. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate system) to give the title compound as a pale yellow oil (0.55 g, 60%).

후처리

  1. washThe mixture was washed with an aqueous saturated ammonium chloride and further brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customevaporated
  4. customThe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate system)

출처 및 근거

ORD 기록
ord-ea03a3065fc448d0a202be055f38092d
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06906072B1

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