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Hydrochloric Acid → HCID 22627680, 화합물

HRID 278060
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HRID 278060 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

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HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 13838HexamethyldisilazaneHCID 13343383HCID 13343383, 화합물HCID 178418339Butyllithium

생성물 1

HCID 22627680HCID 22627680, 화합물

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fc0e2ae39f184b22868b3a1e13a3c2bb
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06359009B1

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