Hydrochloric Acid → Diethyl 2-(1-(4-methoxyphenyl)-2-methylpropan-2-yl)malonate

HRID 1009151

반응식

HRID 1009151 반응식
[CH2:1]([O:3][C:4](=[O:14])[C:5](=[C:11]([CH3:13])[CH3:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].[CH3:15][O:16][C:17]1[CH:25]=[CH:24][C:20]([CH2:21][Mg]Cl)=[CH:19][CH:18]=1.Cl>CCOCC>[CH3:15][O:16][C:17]1[CH:25]=[CH:24][C:20]([CH2:21][C:11]([CH:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])[C:4]([O:3][CH2:1][CH3:2])=[O:14])([CH3:12])[CH3:13])=[CH:19][CH:18]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 81255Diethyl isopropylidenemalonateHCID 178490607HCID 178490607, 화합물

생성물 1

HCID 67304572Diethyl 2-(1-(4-methoxyphenyl)-2-methylpropan-2-yl)malonate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
-78 °C

실험 절차

Diethylisopropylidenemalonate (6.686 ml, 34.09 mmol) was dissolved in 300 ml Et2O and cooled to −78° C. 4-Methoxybenzylmagnesium chloride (150.000 ml, 37.50 mmol) was added and stirring was continued for 5 h. The temperature was warmed up to 0° C. The reaction was hydrolyzed with 0.5 M HCl and extracted 3×EtOAc. Glass col. Chromatography (10-50% EtOAc in Hex.) provided diethyl 2-(1-(4-methoxyphenyl)-2-methylpropan-2-yl)malonate. MS m/z: 323.1 (M+1).

후처리

  1. temperatureThe temperature was warmed up to 0° C
  2. extractionextracted 3×EtOAc

출처 및 근거

ORD 기록
ord-98206daa36f142a3baccedf54bbdc0d0
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973047B2

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