Potassium Carbonate → HCID 22111005, 화합물

HRID 565712노트

반응식

HRID 565712 반응식
I[CH2:2][C:3]1([CH3:18])[CH2:7][C:6]2[C:8]([CH3:17])=[C:9]([NH2:16])[C:10]([CH3:15])=[C:11]([CH:12]([CH3:14])[CH3:13])[C:5]=2[O:4]1.[C:19]1([CH:25]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[NH:26][CH:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C(=O)C.O>[NH2:16][C:9]1[C:10]([CH3:15])=[C:11]([CH:12]([CH3:14])[CH3:13])[C:5]2[O:4][C:3]([CH2:2][N:30]3[CH2:31][CH2:32][CH:27]([NH:26][CH:25]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)[C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH2:28][CH2:29]3)([CH3:18])[CH2:7][C:6]=2[C:8]=1[CH3:17]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 13644890HCID 13644890, 화합물HCID 22111007HCID 22111007, 화합물

생성물 1

HCID 22111005HCID 22111005, 화합물수율 91.9%

시약·촉매·용매 2

HCID 962Water용매HCID 31374Dimethylacetamide용매

실험 절차

A suspension of 2,3-dihydro-2-(iodomethyl)-7-isopropyl-2,4,6-trimethyl-5-benzofuranamine (1.1 g), N-(diphenylmethyl)-4-piperidinamine (1.4 g) and potassium carbonate (0.83 g) in N,N-dimethylacetamide (6 mL) was refluxed for 4.5 hours. The mixture was diluted with water and the product was extracted twice with ethyl acetate. The combined organic layer was washed with water and saturated aqueous sodium chloride, dried over magnesium sulfate, filtrated and evaporated in vacuo. The residue was purified with basic silica gel column chromatography (hexane:ethyl acetate=20:1 to 5:1) and recrystallized from hexane/ethyl acetate to afford 1.4 g of the title compound. Yield 91%.

후처리

  1. temperaturewas refluxed for 4.5 hours
  2. extractionthe product was extracted twice with ethyl acetate
  3. washThe combined organic layer was washed with water and saturated aqueous sodium chloride
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltrated
  6. customevaporated in vacuo
  7. customThe residue was purified with basic silica gel column chromatography (hexane:ethyl acetate=20:1 to 5:1)
  8. customrecrystallized from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-b82d4ca959cc4dc2827767692815f443
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06172085B2

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