Dimethylformamide → HCID 66745583、化合物

HRID 1175756ノート

反応式

HRID 1175756 の反応式
[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

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 8728BromocyclopentaneHCID 11430Potassium CarbonateHCID 16123262HCID 16123262、化合物

生成物 1

HCID 66745583HCID 66745583、化合物

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-904d19f53f264ff99e7643b27883047b
出典データセット
uspto-grants-2010_11
特許番号
US07842703B2

反応ノート

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