Sodium methanethiolate → 2-(4-Chloro-3-methoxyphenyl)-5-trifluoromethyl-3-methylthiopyridine

HRID 1957247ノート

反応式

HRID 1957247 の反応式
Cl[C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([O:19][CH3:20])[CH:13]=2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[CH3:21][S-:22].[Na+]>CO.CN(C)C=O>[Cl:18][C:15]1[CH:16]=[CH:17][C:12]([C:3]2[C:2]([S:22][CH3:21])=[CH:7][C:6]([C:8]([F:11])([F:10])[F:9])=[CH:5][N:4]=2)=[CH:13][C:14]=1[O:19][CH3:20]

参加物

5

反応物 2

HCID 4378561Sodium methanethiolateHCID 157668763-Chloro-2-(4-chloro-3-methoxyphenyl)-5-trifluoromethylpyridine

生成物 1

HCID 190687562-(4-Chloro-3-methoxyphenyl)-5-trifluoromethyl-3-methylthiopyridine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

3.0 g (9.3 mmol) of 3-chloro-2-(4-chloro-3-methoxyphenyl)-5-trifluoromethylpyridine and 0.7 g (10 mmol) of sodium thiomethoxide in a mixture of 50 ml of methanol and 20 ml of dimethylformamide were stirred at 80° C. for 7 h and then at 23° C. for 72 h. The mixture was then poured into 500 ml of ice-water, which was then extracted three times with 150 ml of tert-butyl methyl ether each time. The combined organic phases were washed twice with 100 ml of water each time, dried over sodium sulfate and concentrated.

後処理

  1. waitat 23° C. for 72 h
  2. extractionwas then extracted three times with 150 ml of tert-butyl methyl ether each time
  3. washThe combined organic phases were washed twice with 100 ml of water each time
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-733dc18d305e4a5abf469d33ba1e9ad2
出典データセット
uspto-grants-1998_07
特許番号
US05783522

反応ノート

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