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Methyl iodide → HCID 15292077, 화합물

HRID 1757582
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HRID 1757582 반응식
[CH2:1]([Li])CCC.[CH3:6][C:7]1[N:8]([CH2:33][CH:34]([CH3:36])[CH3:35])[C:9]2[C:14]([CH3:15])=[C:13]([CH3:16])[N:12]=[C:11]([N:17]([CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:10]=2[N:32]=1.CI>O1CCCC1.O.C(OCC)C>[CH2:6]([C:7]1[N:8]([CH2:33][CH:34]([CH3:36])[CH3:35])[C:9]2[C:14]([CH3:15])=[C:13]([CH3:16])[N:12]=[C:11]([N:17]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:25][C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=3)[C:10]=2[N:32]=1)[CH3:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 54167973HCID 54167973, 화합물HCID 178418339Butyllithium

생성물 1

HCID 15292077HCID 15292077, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

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온도
-10 °C

실험 절차

Butyllithium (0.5 mL of 2.5M in hexanes) was added to a cooled (-78°C.) solution of 2,6,7-trimethyl-1-(2-methylpropyl)-N4,N4 -bis(phenylmethyl)-1H-imidazo[4,5-c]pyridin-4-amine (0.5 g, 1.2 mmole) in tetrahydrofuran (30 mL). The reaction mixture was allowed to warm to -10° C. then it was cooled to -78° C. and combined with methyl iodide (0.23 mL, 3.6 mmole). The reaction mixture was allowed to warm to ambient temperature then diluted with water and diethyl ether. Theether layer was separated, washed with ammonium chloride solution, dried over magnesium sulfate and then concentrated to provide 0.5 g of the desired product.

후처리

  1. temperatureit was cooled to -78° C.
  2. temperatureto warm to ambient temperature
  3. customTheether layer was separated
  4. washwashed with ammonium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d3e2575637f24281b89a996b72f6d194
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05446153

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