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Cesium carbonate → 1-(5-Tert-butyl-2-methoxy-3-nitro-phenyl)-pyrrolidin-2-one

HRID 735808
ノート
印刷プレビュー

反応式

HRID 735808 の反応式
Br[C:2]1[CH:7]=[C:6]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[O:15][CH3:16].[NH:17]1[CH2:21][CH2:20][CH2:19][C:18]1=[O:22].C1(P(C2C=CC=CC=2)C2C3OC4C(=CC=CC=4P(C4C=CC=CC=4)C4C=CC=CC=4)C(C)(C)C=3C=CC=2)C=CC=CC=1.C([O-])([O-])=O.[Cs+].[Cs+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:8]([C:6]1[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[C:3]([O:15][CH3:16])=[C:2]([N:17]2[CH2:21][CH2:20][CH2:19][C:18]2=[O:22])[CH:7]=1)([CH3:11])([CH3:10])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 10796Cesium carbonateHCID 120252-PyrrolidoneHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 575500241-Bromo-5-(tert-butyl)-2-methoxy-3-nitrobenzene

生成物 1

HCID 575500321-(5-Tert-butyl-2-methoxy-3-nitro-phenyl)-pyrrolidin-2-one収率 30%

試薬・触媒・溶媒 1

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒

実験手順

An oven-dried Schlenk tube was charged with 2-bromo-4-tert-butyl-6-nitroanisole (500 mg, 1.74 mmol), 2-pyrrolidinone (158 μL, 2.09 mmol), Pd2(dba)3 (32 mg, 0.035 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (58 mg, 0.1 mmol) and Cs2CO3 (795 mg, 2.44 mmol). The tube was capped with a rubber septum, purged with argon and 1,4-dioxane (7 mL) was then added through the septum via a syringe. The tube was sealed with a teflon screwcap, and the reaction mixture was stirred at 100 C for 20 h. The reaction mixture was cooled to room temperature, diluted with EtOAc (100 mL), washed with water, brine and dried over anhydrous Na2SO4. The solvent was removed in vacuo, and crude product was purified by column chromatography (2:1 hexane-EtOAc) to give 1-(5-tert-butyl-2-methoxy-3-nitro-phenyl)-pyrrolidin-2-one (150 mg, 30%).

後処理

  1. customThe tube was capped with a rubber septum
  2. custompurged with argon and 1,4-dioxane (7 mL)
  3. additionwas then added through the septum via a syringe
  4. customThe tube was sealed with a teflon screwcap
  5. additiondiluted with EtOAc (100 mL)
  6. washwashed with water, brine
  7. dry with materialdried over anhydrous Na2SO4
  8. customThe solvent was removed in vacuo, and crude product
  9. customwas purified by column chromatography (2:1 hexane-EtOAc)

出典と根拠

ORDレコード
ord-4af3f91f418340f6ac63231a66db96e2
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592332B2

反応ノート

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