Dimethylformamide → HCID 66745583, 화합물

HRID 1175756노트

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HRID 1175756 반응식
[C:1]12([CH2:9][CH:8](NC(NC3SC4C=C(F)C=CC=4N=3)=O)[C:7]3[CH:24]=[CH:25][CH:26]=[CH:27][C:6]=3[O:5]1)[CH2:4][CH2:3][CH2:2]2.[CH:28]1(Br)C[CH2:31][CH2:30][CH2:29]1.[C:34]([O-:37])([O-])=O.[K+].[K+].CN(C=[O:44])C>>[CH:34]1([O:37][C:25]2[CH:26]=[CH:27][C:6]3[O:5][C:1]4([CH2:2][CH2:3][CH2:4]4)[CH2:9][C:8](=[O:44])[C:7]=3[CH:24]=2)[CH2:31][CH2:30][CH2:29][CH2:28]1

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 8728BromocyclopentaneHCID 11430Potassium CarbonateHCID 16123262HCID 16123262, 화합물

생성물 1

HCID 66745583HCID 66745583, 화합물

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온도
60 °C

실험 절차

To a solution of 3,4-Dihydro-6-hydroxy-4-oxo-spiro[2H-1-benzopyran-2,1′-cyclobutane] (from example 12) (10 mmol) in DMF, cyclopentyl bromide (12 mmol) and K2CO3 (12 mmol) was added and the reaction mixture was heated at 60° C. for 12 h. Solvent was then evaporated and the residue was dissolved in ethyl acetate. Organic layer was washed with water, brine and separated. It was then dried on anhydrous Na2SO4 and concentrated to afford the desired product as oil.

후처리

  1. customSolvent was then evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washOrganic layer was washed with water, brine
  4. customseparated
  5. dry with materialIt was then dried on anhydrous Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-904d19f53f264ff99e7643b27883047b
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07842703B2

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