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6-Bromo-2,2-dimethyl-2H-chromene → 2-(4-benzyloxy-3,5-dimethoxy-phenyl)-1-(2,2-dimethyl-2H-chromen-6-yl)-ethanone

HRID 1724000
ノート
印刷プレビュー

反応式

HRID 1724000 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][C:7]([CH3:13])([CH3:12])[CH:6]=[CH:5]2.[Li]CCCC.[CH2:19]([O:26][C:27]1[C:32]([O:33][CH3:34])=[CH:31][C:30]([CH2:35][CH:36]=[O:37])=[CH:29][C:28]=1[O:38][CH3:39])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C1COCC1>[CH2:19]([O:26][C:27]1[C:32]([O:33][CH3:34])=[CH:31][C:30]([CH2:35][C:36]([C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][CH:11]=2)[O:8][C:7]([CH3:13])([CH3:12])[CH:6]=[CH:5]3)=[O:37])=[CH:29][C:28]=1[O:38][CH3:39])[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 117705336-Bromo-2,2-dimethyl-2H-chromeneHCID 57436872(4-Benzyloxy-3,5-dimethoxy-phenyl)-acetaldehydeHCID 178418339Butyllithium

生成物 1

HCID 575584302-(4-benzyloxy-3,5-dimethoxy-phenyl)-1-(2,2-dimethyl-2H-chromen-6-yl)-ethanone収率 20%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

To a cooled (−78° C.) stirring solution of 6-bromo-2,2-dimethyl-2H-chromene, which was prepared according to Chemistry and Biology, 2000, Vol. 7, p. 979, (567.7 mg, 2.38 mmol) in THF (7 mL) was added n-BuLi (2.88 M, 0.94 mL, 2.71 mmol). After completion of addition, the reaction mixture continued to stir at −78° C. After 25 minutes, (4-benzyloxy-3,5-dimethoxy-phenyl)-acetaldehyde (619.6 mg, 2.17 mmol) dissolved in THF (7.0 mL) was added. After completion of addition the reaction continued to stir for 15 minutes and was then quenched with saturated ammonium chloride. The aqueous layer was separated and extracted with ethyl acetate. All Combined organic layers were dried over sodium sulfate, filtered, and concentrated to yield a crude oil. The crude material was purified by silica gel chromatography (3:1 ethyl acetate:hexanes) to yield the desired product (200.5 mg, 20% yield).

後処理

  1. customwas prepared
  2. additionAfter completion of addition
  3. additionwas added
  4. additionAfter completion of addition the reaction
  5. stirringto stir for 15 minutes
  6. customwas then quenched with saturated ammonium chloride
  7. customThe aqueous layer was separated
  8. extractionextracted with ethyl acetate
  9. dry with materialwere dried over sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customto yield a crude oil
  13. customThe crude material was purified by silica gel chromatography (3:1 ethyl acetate:hexanes)

出典と根拠

ORDレコード
ord-eae5545e2ba14d95830ebe19920ac96b
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07485283B2

反応ノート

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