Potassium Carbonate → 2-n-Butyl-1-pivalyloxymethylimidazole-5-aldehyde

HRID 36992

반응식

HRID 36992 반응식
[CH2:1]([C:5]1[NH:6][C:7]([CH:10]=[O:11])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4].[C:12]([O:18][CH2:19]Cl)(=[O:17])[C:13]([CH3:16])([CH3:15])[CH3:14].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.[O-2].[O-2].[Mn+4]>[CH2:1]([C:5]1[N:6]([CH2:19][O:18][C:12](=[O:17])[C:13]([CH3:16])([CH3:15])[CH3:14])[C:7]([CH:10]=[O:11])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 87885Chloromethyl pivalateHCID 27356712-Butyl-5-formylimidazole

생성물 1

HCID 193873272-n-Butyl-1-pivalyloxymethylimidazole-5-aldehyde

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6228Dimethylformamide용매

실험 절차

A suspension of 2-butylimidazol-5-aldehyde (16,92 g, 0.111 mol, prepared by manganese dioxide oxidation of the alcohol, prepared in Example 1,Method 2), chloromethyl pivalate (21.77 g, 0.145 mol), and potassium carbonate (20.07 g, 0.145 mol) in 200 ml of dimethylformamide was stirred at ambient temperature under argon for four days. The solids were removed by filtration and washed with ether. The combined filtrates were partitioned between diethyl ether and water. The ether phase was washed successively with water and brine, dried over magnesium sulfate and concentrated under vaccum to give 23.6 g of 2-n-butyl-1-pivalyloxymethylimidazole-5-aldehyde.

후처리

  1. customThe solids were removed by filtration
  2. washwashed with ether
  3. customThe combined filtrates were partitioned between diethyl ether and water
  4. washThe ether phase was washed successively with water and brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vaccum

출처 및 근거

ORD 기록
ord-826ff577303045ea8be54312b21db837
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418250

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