Water → 3-Fluoro-4-methylphenyl methyl sulfide

HRID 2380198

반응식

HRID 2380198 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-e634bd928cd6473b8d99d6687553a94c
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05366957

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