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Methyl iodide → HCID 11074136, 화합물

HRID 1904452
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HRID 1904452 반응식
O1CCC[CH2:2]1.[Si]([O:13][C:14]([NH:16][CH:17]([CH2:22][CH:23]=[CH2:24])[C:18]([O:20][CH3:21])=[O:19])=[O:15])(C(C)(C)C)(C)C.CI.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O>[CH3:2][O:13][C:14]([NH:16][CH:17]([CH2:22][CH:23]=[CH2:24])[C:18]([O:20][CH3:21])=[O:19])=[O:15]
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참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 8028Tetrahydrofuran2회HCID 2724141Tetrabutylammonium FluorideHCID 14765842HCID 14765842, 화합물

생성물 1

HCID 11074136HCID 11074136, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

To a tetrahydrofuran solution (3.0 ml) of the compound prepared in Example 3 (170 mg, 0.59 mmol), were successively added dropwise at 0° C. in a nitrogen atmosphere methyl iodide (0.074 ml, 1.18 mmol) and a tetrahydrofuran solution of tetrabutylammonium fluoride (0.59 ml, 0.59 mmol). The mixture was agitated for 1 hour at 0° C., poured into water and extracted with ether. The ether layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under vacuum. The resulting reaction mixture was subjected to column chromatography and eluted with a 1:4 mixture of ether and hexane to give 93 mg of the titled compound (yield, 84% based on the starting materials used in Example 3).

후처리

  1. extractionextracted with ether
  2. dry with materialThe ether layer was dried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under vacuum
  4. customThe resulting reaction mixture
  5. washeluted with a 1:4 mixture of ether and hexane

출처 및 근거

ORD 기록
ord-7a2608409c214c978094489ca36fa32c
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04837349

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