Triethylsilane → HCID 67245862, 화합물

HRID 2425318노트

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HRID 2425318 반응식
[SiH](CC)(CC)CC.[CH2:8]([O:10][C:11](=[O:40])[C:12]([NH:36][C:37](=[O:39])[CH3:38])([CH:18]1[CH2:26][C:25]2[C:20](=[CH:21][CH:22]=[C:23]([CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])[CH:24]=2)[C:19]1=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH3:9]>C(Cl)Cl.Cl[Ti](Cl)(Cl)Cl>[CH2:8]([O:10][C:11](=[O:40])[C:12]([NH:36][C:37](=[O:39])[CH3:38])([CH:18]1[CH2:26][C:25]2[C:20](=[CH:21][CH:22]=[C:23]([CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])[CH:24]=2)[CH2:19]1)[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH3:9]

참가 물질

5

반응물 2

HCID 12052TriethylsilaneHCID 67246761HCID 67246761, 화합물

생성물 1

HCID 67245862HCID 67245862, 화합물수율 72.3%

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매2회

실험 절차

To a solution of Et3SiH (1.014 g, 8.704 mmol) in CH2Cl2 (8 mL) was added 4 (0.213 g, 0.465 mmol) in CH2Cl2 (1.5 mL) dropwise at room temp under N2. TiCl4 (0.354 g, 1.858 mmol) was then added and the reaction left to stir at room temp over night. The reaction was then poured slowly over ice and extracted with CH2Cl2, the organic layer was then dried and concentrated. The product was then purified with silica gel chromatography eluding with 70% hexanes-30% EtOAc. The reaction provided 5 (0.149 g, 0.336 mmol, 72%).

후처리

  1. waitthe reaction left
  2. additionThe reaction was then poured slowly over ice
  3. extractionextracted with CH2Cl2
  4. customthe organic layer was then dried
  5. concentrationconcentrated
  6. customThe product was then purified with silica gel chromatography

출처 및 근거

ORD 기록
ord-d559a71e1a9f4c9a856f4445a8a9955d
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07964649B2

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