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

HRID 1649133노트

반응식

HRID 1649133 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-533ef9704e9945e4adf1ebe5cd346388
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04415579

반응 노트

불러오는 중…