Methyl iodide → Tert-butyl 2-methyl-3-oxobutanoate

HRID 1364506노트

반응식

HRID 1364506 반응식
CI.[C:3]([O-])([O-])=O.[K+].[K+].[O:9]=[C:10]([CH3:19])[CH2:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13]>CC(C)=O>[CH3:3][CH:11]([C:10](=[O:9])[CH3:19])[C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 15538Tert-butyl acetoacetate

생성물 1

HCID 11745089Tert-butyl 2-methyl-3-oxobutanoate수율 56%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Methyl iodide (6.86 mL, 1.1 eq) and K2CO3 (17.97 g, 1.3 eq) were added to an acetone (400 mL) solution of tert-butyl 3-oxobutanoate (15.82 g, 100 mmol) at room temperature. After 15 h, the mixture was filtered and the filtrate was concentrated. The residue was dissolved in ethyl acetate (300 mL), washed with water (30 mL) and brine (300 mL), dried (MgSO4) and concentrated. The crude residue was purified by silica gel chromatography (5-10% EtOAc-hexanes) to give tert-butyl 2-methyl-3-oxobutanoate as a colorless oil (9.56 g, 56%). MS found: (M+Na)+=195.

후처리

  1. filtrationthe mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. dissolutionThe residue was dissolved in ethyl acetate (300 mL)
  4. washwashed with water (30 mL) and brine (300 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe crude residue was purified by silica gel chromatography (5-10% EtOAc-hexanes)

출처 및 근거

ORD 기록
ord-f6cf00c00cf74bbba5243a31f2443d77
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888381B2

반응 노트

불러오는 중…