Sodium Iodide → HCID 67144610, 화합물

HRID 912524

반응식

HRID 912524 반응식
CS([O:5][CH2:6][C:7]1[N:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[CH:10]=[CH:9][CH:8]=1)(=O)=O.O[C:18]1[CH:23]=[CH:22][C:21]([C:24]2[N:29]=[C:28]([C:30]#[N:31])[C:27]3[N:32]=[CH:33][N:34]([CH3:35])[C:26]=3[CH:25]=2)=[CH:20][C:19]=1[C:36]([F:39])([F:38])[F:37].[I-].[Na+].C(=O)([O-])[O-].[K+].[K+]>C(#N)C.O>[C:30]([C:28]1[C:27]2[N:32]=[CH:33][N:34]([CH3:35])[C:26]=2[CH:25]=[C:24]([C:21]2[CH:22]=[CH:23][C:18]([O:5][CH2:6][C:7]3[N:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[CH:10]=[CH:9][CH:8]=3)=[C:19]([C:36]([F:39])([F:38])[F:37])[CH:20]=2)[N:29]=1)#[N:31]

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 54451634Methyl 6-((methylsulfonyloxy)methyl)picolinateHCID 136011085HCID 136011085, 화합물

생성물 1

HCID 67144610HCID 67144610, 화합물수율 78.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

A mixture of methyl 6-((methylsulfonyloxy)methyl)picolinate (733 mg), 6-(4-hydroxy-3-(trifluoromethyl)phenyl)-1-methyl-1H-imidazo[4,5-c]pyridine-4-carbonitrile (950 mg), sodium iodide (44 mg) and potassium carbonate (830 mg) in acetonitrile (20 ml) was heated at 80° C. for 14 hours. After cooling to room temperature, water (30 ml) was added, the white precipitate was collected by filtration and washed with cold methanol (20 ml) to give methyl 6-((4-(4-cyano-1-methyl-1H-imidazo[4,5-c]pyridin-6-yl)-2-(trifluoromethyl)phenoxy)methyl)picolinate (1.1 g). 1H NMR (DMSO) δ: 8.81 (s, 1H), 8.71 (s, 1H), 8.53 (m, 2H), 8.20 (m, 1H), 8.11 (m, 1H), 7.83 (d, 1H), 7.63 (d, 1H), 5.60 (s, 2H), 4.06 (s, 3H), 3.98 (s, 3H). MS m/z 468 (M+1).

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationthe white precipitate was collected by filtration
  3. washwashed with cold methanol (20 ml)

출처 및 근거

ORD 기록
ord-eccf180b5bb34f9e97179b47bbe6c3c1
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026236B2

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