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Diethyl Carbonate → ethyl 6-fluoro-1-(triisopropylsilyl)-1H-indole-5-carboxylate

HRID 336823
ノート
印刷プレビュー

反応式

HRID 336823 の反応式
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[CH:7][N:8]2[Si:11]([CH:18]([CH3:20])[CH3:19])([CH:15]([CH3:17])[CH3:16])[CH:12]([CH3:14])[CH3:13])=[CH:4][CH:3]=1.C([Li])(CC)C.[C:26](=O)([O:30]CC)[O:27][CH2:28][CH3:29].[Cl-].[NH4+]>O1CCCC1>[C:26]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:2]=1[F:1])[N:8]([Si:11]([CH:15]([CH3:17])[CH3:16])([CH:18]([CH3:20])[CH3:19])[CH:12]([CH3:13])[CH3:14])[CH:7]=[CH:6]2)([O:27][CH2:28][CH3:29])=[O:30]
参加物反応条件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 7766Diethyl CarbonateHCID 25517Ammonium ChlorideHCID 117162536-fluoro-1-[tris(propan-2-yl)silyl]-1H-indoleHCID 178418400CID 53628100

生成物 1

HCID 67074085ethyl 6-fluoro-1-(triisopropylsilyl)-1H-indole-5-carboxylate収率 46.9%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
-78 °C

実験手順

To a solution of 760 mg (2.61 mmol) of 6-fluoro-1-triisopropylsilylindole dissolved in 6 ml of anhydrous tetrahydrofuran are added dropwise at −78° C. under argon 2.01 ml of a sec-butyllithium solution (1.3M in cyclohexane, 2.01 mmol). The reaction mixture is stirred for 2 h at −78° C. then 500 μL (3.15 mmol) of diethyl carbonate are added dropwise at −78° C. to the reaction mixture. This mixture is stirred for 5 h with a gentle temperature rise then an ammonium chloride saturated aqueous solution is added. The product is extracted several times with ethyl acetate. The organic phases are combined, dried over magnesium sulfate, and concentrated. The residue is purified by chromatography on silica (cyclohexane/ethyl acetate eluent: 97:3) to yield 445 mg (46%) of 5-carboethoxy-6-fluoro-1-triisopropylsilylindole in the form of a colourless oil.

後処理

  1. stirringThis mixture is stirred for 5 h with a gentle temperature rise
  2. extractionThe product is extracted several times with ethyl acetate
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue is purified by chromatography on silica (cyclohexane/ethyl acetate eluent: 97:3)

出典と根拠

ORDレコード
ord-d65a3426479a4ba0809f4a699a88bc45
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889711B2

反応ノート

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