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Hydrochloric Acid → HCID 22627680、化合物

HRID 278060
ノート
印刷プレビュー

反応式

HRID 278060 の反応式
C[Si](C)(C)N[Si](C)(C)C.[CH2:10]([Li])CCC.[CH:15]([S:18][CH:19]([CH3:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21])([CH3:17])[CH3:16].CI.Cl>O1CCCC1>[CH:15]([S:18][C:19]([CH3:10])([CH3:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21])([CH3:17])[CH3:16]
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 5

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 13838HexamethyldisilazaneHCID 13343383HCID 13343383、化合物HCID 178418339Butyllithium

生成物 1

HCID 22627680HCID 22627680、化合物

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

反応条件

温度
0 °C

実験手順

A solution of 1,1,1,3,3,3-hexamethyldisilazane (10.4 mL, 48 mmol) in tetrahydrofuran is cooled to 0° C., treated with a 2.04 M solution of n-butyllithium in tetrahydrofuran (22.6 mL, 46 mmol), stirred at 0° C. for 30 minutes, treated dropwise with ethyl 2-(isopropylthio)propionate (7.6 g, 42 mmol), stirred at 0° C. for 1 hour, treated with methyl iodide, stirred at room temperature for 22 hours, and poured into an ice-water mixture (100 g) containing 10 mL of 6 N hydrochloric acid. The resultant aqueous mixture is extracted with ether. The combined organic extracts are washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a brown liquid. Vacuum distillation of the brown liquid gives the title product as a liquid (6.8 g) which is identified by NMR spectral analysis.

後処理

  1. stirringstirred at 0° C. for 1 hour
  2. stirringstirred at room temperature for 22 hours
  3. extractionThe resultant aqueous mixture is extracted with ether
  4. washThe combined organic extracts are washed sequentially with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customto obtain a brown liquid
  8. distillationVacuum distillation of the brown liquid

出典と根拠

ORDレコード
ord-fc0e2ae39f184b22868b3a1e13a3c2bb
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06359009B1

反応ノート

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