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(2-Bromoethoxy)-tert-butyldimethylsilane → HCID 68528803、化合物

HRID 2246731
ノート
印刷プレビュー

反応式

HRID 2246731 の反応式
[F:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[N:9]([CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([F:18])[CH:13]=1)[C:8](=[O:19])[C:7]2([CH3:21])[CH3:20].C([Li])CCC.Br[CH2:28][CH2:29][O:30][Si:31]([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:33])[CH3:32]>O1CCCC1>[Si:31]([O:30][CH2:29][CH2:28][CH:11]([N:9]1[C:10]2[C:6](=[CH:5][CH:4]=[CH:3][C:2]=2[F:1])[C:7]([CH3:21])([CH3:20])[C:8]1=[O:19])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([F:18])[CH:13]=1)([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:33])[CH3:32]
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

5

反応物 3

HCID 3608067(2-Bromoethoxy)-tert-butyldimethylsilaneHCID 68528429HCID 68528429、化合物HCID 178418339Butyllithium

生成物 1

HCID 68528803HCID 68528803、化合物収率 55%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
25 °C

実験手順

7-fluoro-1-(3-fluorobenzyl)-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (1.01 g, 3.5 mmol) was dissolved in tetrahydrofuran and cooled to −78° C. n-Butyl lithium (2.5 M in hexane, 1.55 mL, 3.97 mmol) was added dropwise and the mixture was warmed to 0° C. (2-Bromoethoxy)-tert-butyldimethylsilane (1.14 mL, 5.25 mmol) was added and the mixture was allowed to warm to 25° C. The mixture was stirred for 16 hours then quenched with saturated aqueous ammonium chloride, diluted with ether, washed with water, and saturated brine. The organic layer was separated, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The crude product was purified via Isco chromatography (Redisep, silica, gradient 0-10% ethyl acetate in hexane) to afford 0.8 g (55%) 1-[3-{[tert-butyl(dimethyl)silyl]oxy}-1-(3-fluorophenyl)propyl]-7-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one.

後処理

  1. additionwas added dropwise
  2. additionwas added
  3. customthen quenched with saturated aqueous ammonium chloride
  4. additiondiluted with ether
  5. washwashed with water, and saturated brine
  6. customThe organic layer was separated
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe crude product was purified via Isco chromatography (Redisep, silica, gradient 0-10% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-fc971a38b6e4443fa8bdcbd2ba6fc7cb
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07687529B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート