Sodium Hydroxide → 2-({[3-(Trifluoromethyl)phenyl]sulfanyl}methyl)pyridine--hydrogen chloride (1/1)

HRID 1649133ノート

反応式

HRID 1649133 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([SH:9])[CH:6]=[CH:7][CH:8]=1.[OH-].[Na+].Cl.[N:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:21][Cl:22]>C(O)C>[ClH:22].[F:11][C:2]([F:1])([F:10])[C:3]1[CH:4]=[C:5]([S:9][CH2:21][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][N:15]=2)[CH:6]=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 23392Picolyl chloride hydrochlorideHCID 1367513-(Trifluoromethyl)benzenethiol

生成物 1

HCID 129532902-({[3-(Trifluoromethyl)phenyl]sulfanyl}methyl)pyridine--hydrogen chloride (1/1)収率 56%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

m-Trifluoromethylbenzenethiol (5 g) was added to a solution of NaOH (2.25 g) in ethanol (50 ml) and the resulting solution was treated with a solution of 2-picolyl chloride, hydrochloride (4.6 g) in ethanol (25 ml) and the mixture was stirred for 5 hours. The resulting suspension was filtered through kieselghur and the solvent was removed by evaporation. The residue was converted into the hydrochloride in ether with ethereal HCl and recrystallised from acetoneether to give 2-(((3-trifluoromethylphenyl)thio)methyl)pyridine hydrochloride (4.8 g) mp 145°-6° C. Found: C,51.1; H,4.0; N,4.7. C13H10F3NS.HCl requires C,51.0; H,3.6; N,4.6%).

後処理

  1. filtrationThe resulting suspension was filtered through kieselghur
  2. customthe solvent was removed by evaporation
  3. customrecrystallised from acetoneether

出典と根拠

ORDレコード
ord-533ef9704e9945e4adf1ebe5cd346388
出典データセット
uspto-grants-1983_11
特許番号
US04415579

反応ノート

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