2-Methyl-3-buten-2-ol → HCID 22625558, 화합물

HRID 277654노트

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HRID 277654 반응식
[CH3:1][C:2]([OH:6])([CH:4]=[CH2:5])[CH3:3].[CH3:7][Si:8]([SiH:11]([Si:16]([CH3:19])([CH3:18])[CH3:17])[Si:12]([CH3:15])([CH3:14])[CH3:13])([CH3:10])[CH3:9]>N(C1(C#N)CCCCC1)=NC1(C#N)CCCCC1>[CH3:1][C:2]([OH:6])([CH2:4][CH2:5][Si:11]([Si:12]([CH3:15])([CH3:14])[CH3:13])([Si:16]([CH3:19])([CH3:18])[CH3:17])[Si:8]([CH3:7])([CH3:9])[CH3:10])[CH3:3]

참가 물질

4

반응물 2

HCID 82572-Methyl-3-buten-2-olHCID 123134Tris(trimethylsilyl)silane

생성물 1

HCID 22625558HCID 22625558, 화합물수율 75%

시약·촉매·용매 1

HCID 749781,1'-Azobis(cyclohexanecarbonitrile)촉매

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온도
110 °C

실험 절차

A dried reaction flask equipped for magnetic stirring and fitted with a reflux condenser was flushed with nitrogen and charged with toluene (500 mL). Oxygen was purged from the system by passing a stream of nitrogen through the solvent, 2-methyl-3-buten-2-ol (43.1 g, 500 mmol), tris(trimethylsilyl)silane (25.0 g, 100 mmol), and 1,1′-azobis(cyclohexanecarbonitrile) (1.22 g, 5 mmol) were added to the flask, and the reaction mixture was heated for 20 hours at 110° C. with stirring. The resulting solution was concentrated under reduced pressure, and distillation under vacuum (bp 90-104° C. at 0.10 mm) afforded the title compound (25.1 g, 74%) as a colorless solid. The distilled product was characterized by the following NMR data: 1H NMR (CDCl3) δ 0.14 (s, 27 H), 0.70-0.80 (m, 2 H), 1.17 (s, 6 H), 1.30 (br s, 1 H), 1.45-1.55 (m, 2 H); 13C NMR (CDCl3) δ 1.06 (9 C), 1.24 (1 C), 28.35 (2 C), 42.99 (1 C), 71.64 (1 C); 29Si NMR (CDCl3) δ −80.90 (1 Si), −12.83 (3 Si).

후처리

  1. customA dried reaction flask
  2. customequipped
  3. customfitted with a reflux condenser
  4. customwas flushed with nitrogen
  5. additioncharged with toluene (500 mL)
  6. customOxygen was purged from the system
  7. additionwere added to the flask
  8. stirringwith stirring
  9. concentrationThe resulting solution was concentrated under reduced pressure, and distillation under vacuum (bp 90-104° C. at 0.10 mm)

출처 및 근거

ORD 기록
ord-8b9aca523c30479c88171315d03aa37d
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06358675B1

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