ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Nitroethane → HCID 178435547、化合物

HRID 1036468
ノート
印刷プレビュー

反応式

HRID 1036468 の反応式
Br[C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:12][C@H:13]3[CH2:18][CH2:17][C@H:16]([C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:15][CH2:14]3)[CH:8]=2)[CH:3]=1.C(P(C(C)(C)C)C1C=CC=CC=1C1C=CC=CC=1C)(C)(C)C.C(=O)([O-])[O-].[Cs+].[Cs+].COCCOC.[N+:57]([CH2:60][CH3:61])([O-:59])=[O:58]>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]>[C:19]([C@H:16]1[CH2:15][CH2:14][C@H:13]([O:12][C:7]2[CH:6]=[CH:5][C:4]3[C:9](=[CH:10][CH:11]=[C:2]([CH:60]([N+:57]([O-:59])=[O:58])[CH3:61])[CH:3]=3)[CH:8]=2)[CH2:18][CH2:17]1)([CH3:22])([CH3:21])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 6587NitroethaneHCID 80711,2-DimethoxyethaneHCID 10796Cesium carbonateHCID 27349372-(Di-tert-butylphosphino)-2'-methyl-1,1'-biphenylHCID 178445718HCID 178445718、化合物

生成物 1

HCID 178435547HCID 178435547、化合物収率 58%

試薬・触媒・溶媒

1
HCID 6505921(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium触媒

実験手順

A 40 mL vial equipped with a magnetic stir bar was charged with 2-bromo-6-(trans-4-tert-butylcyclohexyloxy)naphthalene (0.6695 g, 1.853 mmol), tris(dibenzylideneacetone)dipalladium(O) (0.06363 g, 0.06948 mmol), 2-(di-t-butylphosphino)-2′-methylbiphenyl (0.08684 g, 0.2779 mmol), and cesium carbonate (0.7245 g, 2.224 mmol). The reaction vessel was capped, evacuated, and backfilled with argon three times then 1,2-dimethoxyethane (20.00 mL, 192.4 mmol) was added via syringe under argon. After the mixture was stirred vigorously for 2 min at room temperature, nitroethane (0.2795 mL, 3.891 mmol) was added and the reaction was heated overnight at 50° C. The reaction was allowed to cool to ambient temperature. The mixture was quenched with a solution of sat. aqueous ammonium chloride. The layers were separated and the aqueous phase was extracted with ethyl acetate. The combined organic phase was washed with water then dried with magnesium sulfate, filtered and concentrated under reduced pressure. The residue was taken up in methylene chloride and silica gel was added. The solvent was removed and the residue was purified by flash column chromatography using 0-20% ethylacetate in hexanes to give the title compound in 58% yield.

後処理

  1. customA 40 mL vial equipped with a magnetic stir bar
  2. customThe reaction vessel was capped
  3. customevacuated
  4. temperaturethe reaction was heated overnight at 50° C
  5. temperatureto cool to ambient temperature
  6. customThe mixture was quenched with a solution of sat. aqueous ammonium chloride
  7. customThe layers were separated
  8. extractionthe aqueous phase was extracted with ethyl acetate
  9. washThe combined organic phase was washed with water
  10. dry with materialthen dried with magnesium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure
  13. additionsilica gel was added
  14. customThe solvent was removed
  15. customthe residue was purified by flash column chromatography

出典と根拠

ORDレコード
ord-bc9a7a3504f04bb09c9e77ff0698af4e
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546359B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート