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Chlorotrimethylsilane → HCID 19974944, 화합물

HRID 1451518
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HRID 1451518 반응식
[CH3:1][Li].C[Si](Cl)(C)C.[Br:8][C:9]1[CH:34]=[CH:33][C:12]([CH2:13][N:14]2[C:22]3[C:17](=[CH:18][C:19]([O:23][CH3:24])=[CH:20][CH:21]=3)[C:16]([CH:25]=[CH:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[C:15]2[CH3:32])=[CH:11][CH:10]=1.[NH4+].[Cl-]>CCOCC.C1COCC1>[Br:8][C:9]1[CH:34]=[CH:33][C:12]([CH2:13][N:14]2[C:22]3[C:17](=[CH:18][C:19]([O:23][CH3:24])=[CH:20][CH:21]=3)[C:16]([CH:25]([CH3:1])[CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[C:15]2[CH3:32])=[CH:11][CH:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6397ChlorotrimethylsilaneHCID 25517Ammonium ChlorideHCID 54298386HCID 54298386, 화합물HCID 178418348HCID 178418348, 화합물

생성물 1

HCID 19974944HCID 19974944, 화합물수율 73.1%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

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온도
-78 °C

실험 절차

To a 0° C. suspension of cuprous iodide (12.7 g, 67.0 mmol) in 150 mL ether was added CH3Li (1.4M in ether, 96 mL, 134 mmol). The solution was cooled to -78° C. and treated with TMSCl (8.5 mL, 67 mmol) and a solution of the unsaturated ester from Step 3 (6.79 g, 15.8 mmol) in 30 mL of THF. The yellow suspension was allowed to warm to room temperature and was stirred 2.5 h. The reaction mixture was poured into saturated NH4Cl and extracted with EtOAc. The organic extracts were washed with water and brine and dried over Na2SO4. Purification by flash chromatography (20% ethyl acetate/hexanes) provided 5.13 g of the title product as a crystaline solid.

후처리

  1. temperatureto warm to room temperature
  2. extractionextracted with EtOAc
  3. washThe organic extracts were washed with water and brine
  4. dry with materialdried over Na2SO4
  5. customPurification by flash chromatography (20% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-cbe3cc555118478e8ebbb18f459c0fba
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05604253

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