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Methyl iodide → 1-[6-Benzyloxy-2-methoxy-3-(5-methyl-7-nitroindan-4-yloxy)phenyl]ethanone

HRID 1766672
ノート
印刷プレビュー

反応式

HRID 1766672 の反応式
[CH2:1]([O:8][C:9]1[C:14]([C:15](=[O:17])[CH3:16])=[C:13]([OH:18])[C:12]([O:19][C:20]2[C:28]([CH3:29])=[CH:27][C:26]([N+:30]([O-:32])=[O:31])=[C:25]3[C:21]=2[CH2:22][CH2:23][CH2:24]3)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:33](=O)([O-])[O-].[Cs+].[Cs+].CI>O1CCCC1>[CH2:1]([O:8][C:9]1[C:14]([C:15](=[O:17])[CH3:16])=[C:13]([O:18][CH3:33])[C:12]([O:19][C:20]2[C:28]([CH3:29])=[CH:27][C:26]([N+:30]([O-:32])=[O:31])=[C:25]3[C:21]=2[CH2:22][CH2:23][CH2:24]3)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 6328Methyl iodideHCID 10796Cesium carbonateHCID 211105611-[6-Benzyloxy-2-hydroxy-3-(5-methyl-7-nitroindan-4-yloxy)phenyl]ethanone

生成物 1

HCID 211105621-[6-Benzyloxy-2-methoxy-3-(5-methyl-7-nitroindan-4-yloxy)phenyl]ethanone収率 98.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 1-[6-benzyloxy-2-hydroxy-3-(5-methyl-7-nitroindan-4-yloxy)phenyl]ethanone (10.0 g) in tetrahydrofuran (15 mL) was added cesium carbonate (7.53 g) under ice-cooling, and then was added dropwise methyl iodide (2.88 mL). After stirring at room temperature overnight, the reaction mixture was evaporated under reduced pressure to dryness. Adding ethyl acetate (30 mL), the mixture was stirred for 30 min. The insoluble material was removed by filtration. The filtrate was evaporated under reduced pressure to dryness to give the title compound (10.2 g).

後処理

  1. temperaturecooling
  2. customthe reaction mixture was evaporated under reduced pressure to dryness
  3. stirringAdding ethyl acetate (30 mL), the mixture was stirred for 30 min
  4. customThe insoluble material was removed by filtration
  5. customThe filtrate was evaporated under reduced pressure to dryness

出典と根拠

ORDレコード
ord-09103b6392d94bcd93a532444372f4f4
出典データセット
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07230031B2

反応ノート

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