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Tributylphosphine → 5-Allyloxy-1-[(2-thiophen-3-yl)ethyl]-1h-indole-2-carboxylic acid ethyl ester

HRID 434017
ノート
印刷プレビュー

反応式

HRID 434017 の反応式
[CH2:1]([O:3][C:4]([C:6]1[NH:7][C:8]2[C:13]([CH:14]=1)=[CH:12][C:11]([O:15][CH2:16][CH:17]=[CH2:18])=[CH:10][CH:9]=2)=[O:5])[CH3:2].[S:19]1[CH:23]=[CH:22][C:21]([CH2:24][CH2:25]O)=[CH:20]1.C(P(CCCC)CCCC)CCC>C1COCC1>[CH2:1]([O:3][C:4]([C:6]1[N:7]([CH2:25][CH2:24][C:21]2[CH:22]=[CH:23][S:19][CH:20]=2)[C:8]2[C:13]([CH:14]=1)=[CH:12][C:11]([O:15][CH2:16][CH:17]=[CH2:18])=[CH:10][CH:9]=2)=[O:5])[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 13831TributylphosphineHCID 83731Thiophene-3-ethanolHCID 13286893Ethyl 5-[(prop-2-en-1-yl)oxy]-1H-indole-2-carboxylate

生成物 1

HCID 120944655-Allyloxy-1-[(2-thiophen-3-yl)ethyl]-1h-indole-2-carboxylic acid ethyl ester収率 94%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To solution of 5-allyloxyindole-2-carboxylic acid ethyl ester (1.0 g, 4.08 mmol) in THF (10 mL) was added azodicarboxylic acid bis[dimethylamide] (TMAD; 1.4 g, 8.15 mmol). After stirring at room temperature for 20 min, 2-(3-thienyl)ethanol (0.78 g, 6.12 mmol) was added followed by the addition of tributyl phosphine (1.65 g, 8.15 mmol). After stirring at room temperature for 18 h, the reaction was partitioned between ethyl acetate and water. The organic layer was washed with brine and dried over Na2SO4. Purification by flash colunmn chromatography (silica gel, EtOAc/hexanes) yielded the desired product as an oil (1.36 g, 94%).

後処理

  1. stirringAfter stirring at room temperature for 18 h
  2. customthe reaction was partitioned between ethyl acetate and water
  3. washThe organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. customPurification by flash colunmn chromatography (silica gel, EtOAc/hexanes)

出典と根拠

ORDレコード
ord-2659ad643eac46948a902f9d8b56e9fb
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06670388B1

反応ノート

読み込み中…

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