反応式
[CH2:1]([C:3]1[C:11]([NH:12][C:13]([CH:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)=[O:14])=[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][N:5]2[N:4]=1)[CH3:2].CC(C)([O-])C.[K+].COCCOC.Br[CH2:34][CH:35]1[CH2:37][CH2:36]1>C1(C)C=CC=CC=1.O>[CH:35]1([CH2:34][N:12]([C:11]2[C:3]([CH2:1][CH3:2])=[N:4][N:5]3[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=23)[C:13]([CH:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)=[O:14])[CH2:37][CH2:36]1参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
A mixture of N4-(2-ethylpyrazolo[1,5-a]pyridin-3-yl)tetrahydro-2H-4-pyrancarboxamide (272 g, 915 mmol), potassium tert-butoxide (144 g, 1.28 mol) and 1,2-dimethoxyethane (1750 mL) was heated and stirred at an external temperature of 40° C. (Bromomethyl)cyclopropane (161 g, 1.19 mol) was then added dropwise to the reaction mixture keeping the internal temperature below 50° C. After heating and stirring for 4 hours, water (1250 mL) and toluene (3750 mL) were added to the reaction mixture. The aqueous layer was removed, and then the organic extract was washed with 10% brine (1250 mL) and water (1250 mL×2 times) in that order, and concentrated under reduced pressure to afford 277 g of the title compound as a brown oil (92.6% yield).
後処理
- temperaturewas heated
- additionwas then added dropwise to the reaction mixture
- customthe internal temperature below 50° C
- temperatureAfter heating
- customThe aqueous layer was removed
- extractionthe organic extract
- washwas washed with 10% brine (1250 mL) and water (1250 mL×2 times) in that order
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-a5055379703f45d2a3b424c54aba9ad6
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07176216B2
関連ノート
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