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Methyl iodide → HCID 178500707, 화합물

HRID 2265911
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HRID 2265911 반응식
[CH3:1][O:2][C:3](=[O:12])[CH2:4][C@H:5]1[CH2:10][CH2:9][C@H:8]([OH:11])[CH2:7][CH2:6]1.[H-].[Na+].I[CH3:16]>CN(C=O)C>[CH3:1][O:2][C:3](=[O:12])[CH2:4][C@H:5]1[CH2:10][CH2:9][C@H:8]([O:11][CH3:16])[CH2:7][CH2:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 178500705HCID 178500705, 화합물

생성물 1

HCID 178500707HCID 178500707, 화합물수율 103.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
2.5 °C

실험 절차

trans-(4-Hydroxy-cyclohexyl)-acetic acid methyl ester (500 mg, 2.90 mmol) were dissolved in 1.5 ml DMF and cooled to 0-5° C. Sodium hydride (190 mg, 4.35 mmol, 55%) and iodomethane (3.62 ml, 23.2 mmol) were added and the reaction mixture stirred for 4 hours at 0-5° C. The reaction mixture was quenched with saturated NaHCO3-solution and extracted with dichloromethane. The organic extract was washed with brine, dried with sodium sulfate, filtered and evaporated. The crude product (561 mg, quant.) was obtained as a colourless oil and used without any further purification for the next step.

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후처리

  1. customThe reaction mixture was quenched with saturated NaHCO3-solution
  2. extractionextracted with dichloromethane
  3. extractionThe organic extract
  4. washwas washed with brine
  5. dry with materialdried with sodium sulfate
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-06257d92765c4b3c875cfcf11d6f00ca
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858630B2

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