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Lithium hexamethyldisilazane → 1-(3-Bromo-4-fluorophenyl)-2-[4-(2-fluoroethoxy)-phenyl]ethane-1,2-dione

HRID 643481
ノート
印刷プレビュー

反応式

HRID 643481 の反応式
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[Br-].[Br:12][C:13]1[CH:14]=[C:15]([CH:36]=[CH:37][C:38]=1[F:39])[CH2:16][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[F:40][CH2:41][CH2:42][O:43][C:44]1[CH:52]=[CH:51][C:47]([C:48](Cl)=[O:49])=[CH:46][CH:45]=1.I([O-])(=O)(=O)=[O:54].[Na+]>O1CCCC1.O>[Br:12][C:13]1[CH:14]=[C:15]([C:16](=[O:54])[C:48]([C:47]2[CH:51]=[CH:52][C:44]([O:43][CH2:42][CH2:41][F:40])=[CH:45][CH:46]=2)=[O:49])[CH:36]=[CH:37][C:38]=1[F:39]
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

7

反応物 4

HCID 2733832Lithium hexamethyldisilazaneHCID 23667635Sodium periodateHCID 450818234-(2-Fluoroethoxy)benzoyl chlorideHCID 86602228(3-Bromo-4-fluoro-benzyl)triphenylphosphonium bromide

生成物 1

HCID 575312621-(3-Bromo-4-fluorophenyl)-2-[4-(2-fluoroethoxy)-phenyl]ethane-1,2-dione収率 41%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
-20 °C

実験手順

A 1.0 M solution of lithium bis(trimethylsilyl)amide in tetrahydrofuran (20 mL, 20 mmol was added at room temperature to a stirred suspension of (3-bromo-4-fluoro-benzyl)triphenylphosphonium bromide (10.6 g, 20 mmol) in tetrahydrofuran (40 mL). The mixture was stirred for 40 minutes, then cooled to −20° C. and treated with 4-(2-fluoroethoxy)benzoyl chloride (4.1 g, 20 mmol) in tetrahydrofuran (40 mL) and stirred for an additional 2 hours while slowly warming to room temperature. The mixture was treated with water (20 mL) and sodium periodate (4.3 g, 20 mmol) then stirred at 50° C. for 18 hours. After cooling to room temperature the mixture was extracted with ethyl acetate. The organic extracts were washed with brine, dried over MgSO4. Evaporation and purification by flash chromatography (hexane/ethyl acetate 9/1) gave a yellow solid (3 g, 41% yield); 1H NMR (400 MHZ, CDCl3) δ 4.25 (m, 1H), 4.32 (m, 1H,) 4.70 (m, 1H), 4.82 (m, 1H), 7.01 (d, 2H), 7.23 (m, 1H), 7.94 (m, 3H), 8.22 (m, 1H); MS m/e (M+CH3COO)− 427; mp 107° C.

後処理

  1. stirringstirred for an additional 2 hours
  2. temperaturewhile slowly warming to room temperature
  3. stirringthen stirred at 50° C. for 18 hours
  4. temperatureAfter cooling to room temperature the mixture
  5. extractionwas extracted with ethyl acetate
  6. washThe organic extracts were washed with brine
  7. dry with materialdried over MgSO4
  8. customEvaporation and purification by flash chromatography (hexane/ethyl acetate 9/1)

出典と根拠

ORDレコード
ord-48d9a0e0211e4e77837da9b4bc2c7e48
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07700602B2

反応ノート

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