Water → 3-Fluoro-4-methylphenyl methyl sulfide

HRID 21451

反応式

HRID 21451 の反応式
[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]

参加物

6

反応物 4

HCID 962WaterHCID 99573-Fluoro-4-methylaniline2 回HCID 10906Tert-Butyl nitrite2 回HCID 12232Dimethyl Disulfide

生成物 1

HCID 534144923-Fluoro-4-methylphenyl methyl sulfide収率 525.5%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9b753ec268a24204821843de40f5cfd5
出典データセット
uspto-grants-1995_06
特許番号
US05424276

関連ノート

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