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Pentane → 3-bromo-1-(tert-butyl-dimethyl-silanyl)-6-(tert-butyl-dimethyl-silanyloxy)-1H-indole

HRID 1767934
ノート
印刷プレビュー

反応式

HRID 1767934 の反応式
[Li]CCCC.CCCCC.[C:11]([Si:15]([CH3:27])([CH3:26])[O:16][C:17]1[CH:25]=[C:24]2[C:20]([CH:21]=[CH:22][NH:23]2)=[CH:19][CH:18]=1)([CH3:14])([CH3:13])[CH3:12].[Si:28](Cl)([C:31]([CH3:34])([CH3:33])[CH3:32])([CH3:30])[CH3:29].[Br:36]N1C(=O)CCC1=O>C1COCC1.C(OCC)C>[Br:36][C:21]1[C:20]2[C:24](=[CH:25][C:17]([O:16][Si:15]([C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:27])[CH3:26])=[CH:18][CH:19]=2)[N:23]([Si:28]([C:31]([CH3:34])([CH3:33])[CH3:32])([CH3:30])[CH3:29])[CH:22]=1
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

8

反応物 5

HCID 8003PentaneHCID 28928tert-Butyldimethylsilyl chlorideHCID 67184N-bromobutanimideHCID 222508166-((tert-butyldimethylsilyl)oxy)-1H-indoleHCID 178418339Butyllithium

生成物 1

HCID 236144903-bromo-1-(tert-butyl-dimethyl-silanyl)-6-(tert-butyl-dimethyl-silanyloxy)-1H-indole
収率 74.1%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

A 1.6 M solution of BuLi in pentane (6.57 ml, 10.5 mmol) was added to a solution of 6-(tert-butyl-dimethyl-silanyloxy)-1H-indole (2 g, 8.1 mmol) in THF (40 ml) at −78° C. within 20 min under an argon atmosphere. The reaction mixture was stirred for 20 min at −78° C. tert-Butyldimethylsilyl chloride (1.6 g, 10.5 mmol) was added and the reaction mixture was stirred for 10 min at −78° C. and for 1 h at RT. The mixture was chilled to −78° C., N-bromosuccinimide (1.6 g, 8.9 mmol) was added and stirring was continued for 1 h at −78° C. and for 1 h at RT. The solution was diluted with diethyl ether and washed with saturated aqueous NaHCO3 solution and water. The ether phase was dried over sodium sulfate, concentrated under reduced pressure and the residue was purified by column chromatography (silica gel, n-heptane/ethyl acetate 1:19) to give 2.64 g (6 mmol, 74%) 3-bromo-1-(tert-butyl-dimethyl-silanyl)-6-(tert-butyl-dimethyl-silanyloxy)-1H-indole as brown solid.

後処理

  1. additionwas added
  2. temperatureThe mixture was chilled to −78° C.
  3. stirringstirring
  4. waitwas continued for 1 h at −78° C. and for 1 h at RT
  5. washwashed with saturated aqueous NaHCO3 solution and water
  6. dry with materialThe ether phase was dried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customthe residue was purified by column chromatography (silica gel, n-heptane/ethyl acetate 1:19)

出典と根拠

ORDレコード
ord-5b8ffa335ac7487fbc625e8eec87e620
出典データセット
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07235572B2

反応ノート

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