3-(2-fluoro-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole → 3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole

HRID 1020946노트

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HRID 1020946 반응식
[O:1]([CH3:3])[K].CO.C1(C)C=CC=CC=1.F[C:14]1[CH:19]=[C:18]([C:20]2[C:28]3[C:23](=[CH:24][CH:25]=[C:26]([N+:29]([O-:31])=[O:30])[CH:27]=3)[N:22]([C:32]([C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=3)([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[N:21]=2)[CH:17]=[CH:16][N:15]=1>>[CH3:3][O:1][C:14]1[CH:19]=[C:18]([C:20]2[C:28]3[C:23](=[CH:24][CH:25]=[C:26]([N+:29]([O-:31])=[O:30])[CH:27]=3)[N:22]([C:32]([C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=3)([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[N:21]=2)[CH:17]=[CH:16][N:15]=1

참가 물질

3

반응물 2

HCID 583719213-(2-fluoro-pyridin-4-yl)-5-nitro-1-trityl-1H-indazoleHCID 178501899HCID 178501899, 화합물

생성물 1

HCID 673446273-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole수율 100%

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온도
70 °C

실험 절차

In a 250 ml pressure vessel, 3-(2-Fluoro-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole 3BV (5.005 g, 10.0 mmole) was dissolved in 0.1N KOCH3/MeOH/Toluene (Acros, 150 mL, 15.0 mmole) under dry N2 gas. The pressure vessel was tightly sealed and heated under stirring at 70° C. for 24 hours. The pressure vessel was cooled to 0° C. in ice-bath before opening. The contents of the pressure vessel were transferred to 500 ml RBF and evaporated to dryness. The resulting solid was dissolved in CH2Cl2 and washed with saturated NaCl solution and dried over MgSO4. The solvent was evaporated to dryness and dried under high vacuum to yield 4BV as a brown solid (5.12 g, 100%).

후처리

  1. customThe pressure vessel was tightly sealed
  2. temperatureheated
  3. temperatureThe pressure vessel was cooled to 0° C. in ice-bath
  4. customevaporated to dryness
  5. dissolutionThe resulting solid was dissolved in CH2Cl2
  6. washwashed with saturated NaCl solution
  7. dry with materialdried over MgSO4
  8. customThe solvent was evaporated to dryness
  9. customdried under high vacuum

출처 및 근거

ORD 기록
ord-3ec114f409f8495abaa60812f278037e
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716483B2

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