Hydrochloric Acid → HCID 54428804、化合物

HRID 341735

反応式

HRID 341735 の反応式
N([O-])=O.[Na+].[Cl:5][C:6]1[C:12]([CH3:13])=[CH:11][CH:10]=[C:9]([Cl:14])[C:7]=1N.Cl.[CH3:16][S:17]SC>O.C(O)(=O)C.[Cu]>[Cl:5][C:6]1[C:7]([S:17][CH3:16])=[C:9]([Cl:14])[CH:10]=[CH:11][C:12]=1[CH3:13]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 12232Dimethyl DisulfideHCID 1165292,6-Dichloro-3-methylanilineHCID 23668193Sodium Nitrite

生成物 1

HCID 54428804HCID 54428804、化合物

試薬・触媒・溶媒 3

HCID 23978Copper触媒HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

A solution of sodium nitrite (12.0 g) in water was added to a stirred suspension of 2,6-dichloro-3-methylaniline (30.0 g) in a mixture of glacial acetic acid and concentrated hydrochloric acid. While maintaining the temperature below 10° C. The mixture was stirred at 0° C. for three quarters of an hour then added to a mixture of dimethyl disulphide (20 ml) and copper powder (0.25 g) in glacial acetic acid. The mixture was stirred for 4 hours and extracted with ether. The organic layer was washed with aqueous sodium carbonate (2M), water, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness to give 2,4-dichloro-3-(methylsulphenyl)toluene (27.2 g) as a red liquid NMR (CDCl3) 2.4(s,3H), 2.45(s,3H), 7.15(d,1H), 7.3(d,1H).

後処理

  1. temperatureWhile maintaining the temperature below 10° C
  2. stirringThe mixture was stirred for 4 hours
  3. extractionextracted with ether
  4. washThe organic layer was washed with aqueous sodium carbonate (2M), water
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness

出典と根拠

ORDレコード
ord-b8985a846b5a4156bb3bc733b0afee4a
出典データセット
uspto-grants-1999_01
特許番号
US05856274

関連ノート

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