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Methyl iodide → HCID 22063735, 화합물

HRID 1828463
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HRID 1828463 반응식
[OH:1][CH2:2]/[CH:3]=[CH:4]/[C:5]1[C:10](=[O:11])[N:9]2[CH:12]=[CH:13][C:14]([CH2:16][CH2:17][C:18]3[S:19][CH:20]=[C:21]([CH:23]([CH3:25])[CH3:24])[N:22]=3)=[CH:15][C:8]2=[N:7][C:6]=1[N:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1.[CH2:32]([Zn]CC)C.CCCCCC.IC.[Cl-].[NH4+]>ClCCl>[OH:1][CH2:2][CH:3]1[CH2:32][CH:4]1[C:5]1[C:10](=[O:11])[N:9]2[CH:12]=[CH:13][C:14]([CH2:16][CH2:17][C:18]3[S:19][CH:20]=[C:21]([CH:23]([CH3:25])[CH3:24])[N:22]=3)=[CH:15][C:8]2=[N:7][C:6]=1[N:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1
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참가 물질

7

반응물 5

HCID 6328Methyl iodideHCID 8058HexaneHCID 25517Ammonium ChlorideHCID 22063619HCID 22063619, 화합물HCID 178418750HCID 178418750, 화합물

생성물 1

HCID 22063735HCID 22063735, 화합물수율 73%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

3-[(E)-3-Hydroxy-1-propenyl]-8-[2-(4-isopropyl-1,3-thiazol-2-yl)ethyl]-2-morpholino-4H-pyrido[1,2-a]pyrimidin-4-one (81 mg, 0.18 mmol) was added with dichloromethane (3 ml) and a solution of diethyl zinc in hexane (1.02 M, 270 μl, 0.275 mmol) and subsequently added dropwise with iodomethane (30 μl, 0.366 mmol) at room temperature. After the reaction solution was stirred for 2 hours, the reaction was stopped with saturated aqueous ammonium chloride, and the reaction solution was extracted with chloroform. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by thin layer silica gel chromatography (chloroform:methanol=15:1) to obtain 61 mg (73%) of the title compound.

후처리

  1. extractionthe reaction solution was extracted with chloroform
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by thin layer silica gel chromatography (chloroform:methanol=15:1)

출처 및 근거

ORD 기록
ord-736d77570e624b119e0d0cd7b3bde43e
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07056917B2

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