Hydrochloric Acid → HCID 54428804, 화합물

HRID 341735

반응식

HRID 341735 반응식
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]

참가 물질

8

반응물 4

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

생성물 1

HCID 54428804HCID 54428804, 화합물

시약·촉매·용매 3

HCID 23978Copper촉매HCID 176Acetic Acid용매2회HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b8985a846b5a4156bb3bc733b0afee4a
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856274

연결된 노트

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