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Methanol → HCID 69522772, 화합물

HRID 1181446
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HRID 1181446 반응식
[H-].[Na+].[CH:3]1[C:12]2[C:7](=[C:8]([NH:13][C:14]([NH:16][CH2:17][C:18]3[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][CH:19]=3)=[O:15])[CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][N:4]=1.[CH3:28]I.CO>C1COCC1.C(Cl)Cl>[CH:3]1[C:12]2[C:7](=[C:8]([N:13]([CH3:28])[C:14]([NH:16][CH2:17][C:18]3[CH:23]=[CH:22][C:21]([C:24]([F:25])([F:26])[F:27])=[CH:20][CH:19]=3)=[O:15])[CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 887MethanolHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 8068410A-425619

생성물 1

HCID 69522772HCID 69522772, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028
Tetrahydrofuran
용매

실험 절차

Sodium hydride (60% dispersion in oil, 7 mg, 0.17 mmol) was added to a suspension N-isoquinolin-5-yl-N′-[4-(trifluoromethyl)benzyl]urea (Example 14; 48 mg, 0.14 mmol) in THF (3 mL) at room temperature and the reaction was stirred until effervescence ceased (20 minutes). Methyl iodide (11 μL, 0.17 mmol) was added and the reaction stirred at room temperature for 3 hours. TLC analysis (10% MeOH in CH2Cl2) indicated only one major product. The reaction was evaporated in vacuo and the product isolated by preparative TLC (4% MeOH in CH2Cl2) to give the title compound. m/z (ES+) 360 (M+H)+.

후처리

  1. custom(20 minutes)
  2. stirringthe reaction stirred at room temperature for 3 hours
  3. customThe reaction was evaporated in vacuo
  4. customthe product isolated by preparative TLC (4% MeOH in CH2Cl2)

출처 및 근거

ORD 기록
ord-fc8d90e57832447e86951084d3bdb318
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07285563B2

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