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Sodium Sulfate → HCID 10728422, 화합물

HRID 2396258
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HRID 2396258 반응식
[CH:1]([C:4]1[CH:12]=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:10]=[C:9]([CH:16]([CH3:18])[CH3:17])[C:5]=1[C:6](Cl)=[O:7])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[O-]S([O-])(=O)=O.[Na+].[Na+]>CCOCC>[CH:16]([C:9]1[CH:10]=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:12]=[C:4]([CH:1]([CH3:3])[CH3:2])[C:5]=1[CH2:6][OH:7])([CH3:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 926972,4,6-Triisopropylbenzoyl chlorideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 10728422HCID 10728422, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of commercially available 2,4,6-triisopropylbenzoyl chloride (35g, 131.2 mmol) in 400 mL ether was added slowly to a suspension of lithium aluminum hydride (LAH) (4.89 g, 131.2 mmol) in ether (300 mL) at -15° C. The mixture was slowly warmed to room temperature over 18 hours. Saturated Na2SO4 solution was added slowly and the etherlayer was separated, dried over MgSO4, and evaporated to dryness. The compound was used in the next step without further purification; NMR (CDCl3): δ 1.2-1.4 (m, 18H), 2.8-3.0 (m, 1H), 3.3-3.5 (m, 2H), 4.8 (s, 2H), 7.1 (s, 2H) ppm.

후처리

  1. customthe etherlayer was separated
  2. dry with materialdried over MgSO4
  3. customevaporated to dryness
  4. customThe compound was used in the next step without further purification

출처 및 근거

ORD 기록
ord-ba97f10fd49e46249842a3dedb3a494f
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05491172

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