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Methyl iodide → KF-17837

HRID 1077447
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HRID 1077447 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:25]=[CH:26][C:27]=1[O:28][CH3:29])/[CH:6]=[CH:7]/[C:8]1[NH:16][C:15]2[C:14](=[O:17])[N:13]([CH2:18][CH2:19][CH3:20])[C:12](=[O:21])[N:11]([CH2:22][CH2:23][CH3:24])[C:10]=2[N:9]=1.[C:30](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:25]=[CH:26][C:27]=1[O:28][CH3:29])/[CH:6]=[CH:7]/[C:8]1[N:16]([CH3:30])[C:15]2[C:14](=[O:17])[N:13]([CH2:18][CH2:19][CH3:20])[C:12](=[O:21])[N:11]([CH2:22][CH2:23][CH3:24])[C:10]=2[N:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 10475986HCID 10475986, 화합물

생성물 1

HCID 6448585KF-17837수율 98%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Compound B (1.20 g, 3.02 mmol) was dissolved in 20 ml of dimethylformamide. To the solution were added 1.04 g (7.55 mmol) of potassium carbonate and subsequently 0.38 ml (6.04 mmol) of methyl iodide, and the resultant mixture was stirred at 50° C. for 30 minutes. After cooling, insoluble matters were filtered off, and 400 ml of water was added to the filtrate. The mixture was extracted three times with 100 ml of chloroform. The extract was washed twice with water and once with a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (eluent: 1% methanol/chloroform), followed by recrystallization from propanol/water to give 1.22. g (yield 98%) of Compound 1 as white needles.

후처리

  1. temperatureAfter cooling
  2. filtrationinsoluble matters were filtered off
  3. addition400 ml of water was added to the filtrate
  4. extractionThe mixture was extracted three times with 100 ml of chloroform
  5. washThe extract was washed twice with water and once with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous sodium sulfate
  7. customfollowed by evaporation under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (eluent: 1% methanol/chloroform)
  9. customfollowed by recrystallization from propanol/water
  10. customto give 1.22

출처 및 근거

ORD 기록
ord-76a340c5a42a4103883e3203b6e2778f
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05543415

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