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2-Bromo-2-methylpropanoyl cyanide → 5-(4-(benzyloxy)phenyl)-4-(4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one

HRID 655369
ノート
印刷プレビュー

反応式

HRID 655369 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=[O:25])[CH2:16][C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC([O-])(C)C.[K+].Br[C:33]([CH3:39])([CH3:38])[C:34](C#N)=[O:35]>C1COCC1>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[O:25][C:33]([CH3:39])([CH3:38])[C:34](=[O:35])[C:16]=2[C:17]2[CH:18]=[CH:19][C:20]([O:23][CH3:24])=[CH:21][CH:22]=2)=[CH:11][CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物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 124878382-Bromo-2-methylpropanoyl cyanideHCID 189237831-(4-(Benzyloxy)phenyl)-2-(4-methoxyphenyl)ethanoneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 593547815-(4-(benzyloxy)phenyl)-4-(4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one収率 4.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a pre-cooled 0° C. solution of 1-(4-(benzyloxy)phenyl)-2-(4-methoxyphenyl)-ethanone (2 g, 6.02 mmol) in THF (20 mL) under an inert atmosphere was added t-BuOK (8 mL, 1.0 N solution in THF). The mixture was then stirred for 30 minutes. 2-Bromo-2-methylpropanoyl cyanide (2 g, 12 mmol) was then added to then reaction mixture and stirring was continued for an additional 16 h. The reaction mixture was then quenched with cold water (10 mL) and extracted with EtOAc (2×50 mL). The combined organic layers were washed with water (30 mL) and brine (30 mL), and then dried over Na2SO4 concentrated and purified via silica gel column chromatography (10-15% Ethyl acetate in hexanes) to afford 5-(4-(benzyloxy)phenyl)-4-(4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one (100 mg) as a white solid.

後処理

  1. customreaction mixture
  2. stirringstirring
  3. waitwas continued for an additional 16 h
  4. customThe reaction mixture was then quenched with cold water (10 mL)
  5. extractionextracted with EtOAc (2×50 mL)
  6. washThe combined organic layers were washed with water (30 mL) and brine (30 mL)
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated
  9. custompurified via silica gel column chromatography (10-15% Ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-5d46e2f4302c4990aaf4a81c197284aa
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071595B2

反応ノート

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