Methyl iodide → HCID 59487515, 화합물

HRID 886715노트

반응식

HRID 886715 반응식
[OH:1][CH:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]=[O:12])[C:5]=2[C:4](=[O:13])[O:3]1.[C:14](=O)([O-])[O-].[K+].[K+].IC>CN(C)C=O>[CH:2]([C:6]1[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]=[O:12])[C:5]=1[C:4]([O:3][CH3:14])=[O:13])=[O:1]

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 11430Potassium CarbonateHCID 12746936HCID 12746936, 화합물

생성물 1

HCID 59487515HCID 59487515, 화합물수율 83%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1-hydroxy-3-oxo-1,3-dihydro-2-benzofuran-4-carbaldehyde (720 mg) in anhydrous dimethylformamide (4 ml) was added potassium carbonate (613 mg). It was stirred for 30 minutes to give a thick white suspension. Iodomethane (0.4 ml) was added and stirred for 3 days. More methyl iodide (0.4 ml) was added and stirring continued for 24 hours. Most of the dimethylformamide was evaporated in vacuo. The pale yellow residue was partitioned between ethyl acetate (25 ml) and water (25 ml) and the organic phase was washed with aqueous lithium chloride (50 ml) and saturated brine (25 ml), dried over sodium sulphate and evaporated to give a pale yellow solid (645 mg).

후처리

  1. customto give a thick white suspension
  2. stirringstirred for 3 days
  3. stirringstirring
  4. waitcontinued for 24 hours
  5. customMost of the dimethylformamide was evaporated in vacuo
  6. customThe pale yellow residue was partitioned between ethyl acetate (25 ml) and water (25 ml)
  7. washthe organic phase was washed with aqueous lithium chloride (50 ml) and saturated brine (25 ml)
  8. dry with materialdried over sodium sulphate
  9. customevaporated

출처 및 근거

ORD 기록
ord-069fc82789544708bfdfed9bc6f73a62
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247377B2

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