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Iodoethane → HCID 9836705、化合物

HRID 1057364
ノート
印刷プレビュー

反応式

HRID 1057364 の反応式
[C:1]([O:5][C:6]([CH:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[CH:16][C:17]([O:19][CH3:20])=[CH:18][C:11]=2[NH:10][C:9]1=[O:21])=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:22](I)[CH3:23].C([O-])([O-])=O.[Cs+].[Cs+]>C(#N)C>[C:1]([O:5][C:6]([CH:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[CH:16][C:17]([O:19][CH3:20])=[CH:18][C:11]=2[N:10]([CH2:22][CH3:23])[C:9]1=[O:21])=[O:7])([CH3:4])([CH3:3])[CH3:2]
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 6340IodoethaneHCID 10796Cesium carbonateHCID 9857210HCID 9857210、化合物

生成物 1

HCID 9836705HCID 9836705、化合物収率 88%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A suspension of 3(R,S)-tert-butoxycarbonyl-8-methoxy-2,3,4,5-tetrahydro-1H-1-benzazepine-2-one (3.645 g, 12.51 mmol), ethyl iodide (2.01 mL, 25.02 mmol) and Cs2CO3 (8.153 g, 25.02 mmol) in acetonitrile (35 mL) was stirred at room temperature for 6 hrs. The reaction mixture was evaporated to dryness, the residue dissolved in water and extracted with DCM. The organic layer was washed with water, dried over Na2SO4, filtered and evaporated to dryness. The solid residue was washed with n-hexane and dried in vacuum. The desired compound (3.50 g, 88%) was obtained as white crystalline powder.

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionthe residue dissolved in water
  3. extractionextracted with DCM
  4. washThe organic layer was washed with water
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness
  8. washThe solid residue was washed with n-hexane
  9. customdried in vacuum

出典と根拠

ORDレコード
ord-156503904e64450f998d2edcc2d98a94
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06514965B1

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