Water → 6-(2-Fluoro-4-trifluoromethyl-phenyl)-2-methyl-3-[4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-pyridine

HRID 33547노트

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HRID 33547 반응식
[N:1]1([CH2:6][CH2:7][CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH:5]=[CH:4][N:3]=[N:2]1.[H-].[Na+].Cl[CH2:20][C:21]1[C:22]([CH3:38])=[N:23][C:24]([C:27]2[CH:32]=[CH:31][C:30]([C:33]([F:36])([F:35])[F:34])=[CH:29][C:28]=2[F:37])=[CH:25][CH:26]=1.O>CN(C)C=O>[F:37][C:28]1[CH:29]=[C:30]([C:33]([F:35])([F:36])[F:34])[CH:31]=[CH:32][C:27]=1[C:24]1[N:23]=[C:22]([CH3:38])[C:21]([CH2:20][O:16][C:13]2[CH:12]=[CH:11][C:10]([CH2:9][CH2:8][CH2:7][CH2:6][N:1]3[CH:5]=[CH:4][N:3]=[N:2]3)=[CH:15][CH:14]=2)=[CH:26][CH:25]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 121094944-(4-[1,2,3]Triazol-1-yl-butyl)phenolHCID 69106508HCID 69106508, 화합물

생성물 1

HCID 160653056-(2-Fluoro-4-trifluoromethyl-phenyl)-2-methyl-3-[4-(4-[1,2,3]triazol-1-yl-butyl)-phenoxymethyl]-pyridine수율 77.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

A solution of 359 mg (1.65 mmol) 4-(4-[1,2,3]triazol-1-yl-butyl)phenol in 20.0 ml N,N-dimethylformamide was treated at 0° C. with 66 mg (1.65 mmol) of 60% sodium hydride and stirred at 0° C. for 30 min. Then 500 mg (1.65 mmol) 3-Chloromethyl-6-(2-fluoro-4-trifluoromethyl-phenyl)-2-methyl-pyridine were added and stirred continued at r. t. over night. After addition of 40 ml water, the precipitate was isolated, washed thoroughly with water and diisopropylether. The residue was dried at 40° C. to give 618 mg (77%) of the title compound as light brown powder.

후처리

  1. stirringstirred
  2. waitover night
  3. customthe precipitate was isolated
  4. washwashed thoroughly with water and diisopropylether
  5. customThe residue was dried at 40° C.

출처 및 근거

ORD 기록
ord-7be83fbf10a04239855bafcd232f56ee
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429605B2

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