Water → 3-Fluoro-4-methylphenyl methyl sulfide

HRID 21451

반응식

HRID 21451 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[CH3:9])N.[CH3:10][S:11]SC.N(OC(C)(C)C)=O.O>ClCCCl>[F:1][C:2]1[CH:3]=[C:4]([S:11][CH3:10])[CH:6]=[CH:7][C:8]=1[CH3:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 99573-Fluoro-4-methylaniline2회HCID 10906Tert-Butyl nitrite2회HCID 12232Dimethyl Disulfide

생성물 1

HCID 534144923-Fluoro-4-methylphenyl methyl sulfide수율 525.5%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매2회

실험 절차

A mixture of 3-fluoro-4-methylaniline (25 g), dimethyl disulphide (375 g) and t-butyl nitrite (30 ml) in 1,2-dichloroethane was warmed to start the reaction. A solution of 3-fluoro-4-methylaniline (225 g) in 1,2-dichloroethane was added dropwise, simultaneously with t-butyl nitrite (241 ml) at such a rate as to maintain the temperature below 60° C. The mixture was stirred for 2 hours, then water was added. The organic layer was washed with water, hydrochloric acid, dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 2-fluoro-4-(methylsulphenyl)toluene (164 g) as a yellow oil; NMR (acetone-d6); 2.2 (3H,d), 2.5 (3H,s), 7.05 (3H,m).

후처리

  1. temperaturewas warmed
  2. customthe reaction
  3. temperatureto maintain the temperature below 60° C
  4. washThe organic layer was washed with water, hydrochloric acid
  5. dry with materialdried (anhydrous magnesium sulphate)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness
  8. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-9b753ec268a24204821843de40f5cfd5
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424276

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