Tert-Butyl nitrite → Benzene, 1-bromo-2-(methylthio)-4-(trifluoromethyl)-

HRID 21462

반응식

HRID 21462 반응식
N(OC(C)(C)C)=O.N[C:9]1[CH:10]=[C:11]([C:16]([F:19])([F:18])[F:17])[CH:12]=[CH:13][C:14]=1[Br:15].[CH3:20][S:21]SC>C(Cl)(Cl)Cl>[Br:15][C:14]1[CH:13]=[CH:12][C:11]([C:16]([F:19])([F:18])[F:17])=[CH:10][C:9]=1[S:21][CH3:20]

참가 물질

5

반응물 3

HCID 10906Tert-Butyl nitrite2회HCID 12232Dimethyl DisulfideHCID 679892-Bromo-5-(trifluoromethyl)benzenamine2회

생성물 1

HCID 11000144Benzene, 1-bromo-2-(methylthio)-4-(trifluoromethyl)-

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

t-Butyl nitrite (3 ml) was added to a mixture of 3-amino-4-bromobenzotrifluoride (4 g) and dimethyl disulphide (15 ml) in chloroform. The mixture was warmed until reaction started when t-butyl nitrite (11 ml) and a solution of 3-amino-4-bromobenzotrifluoride (16 g) in chloroform were added simultaneously. The resultant mixture was stirred for 24 hours, washed with water, hydrochloric acid (2M), water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 4-bromo-3-(methylsulphenyl)benzotrifluoride (16.4 g) as a yellow oil, b.p. 84°-88° C. at 2 mm Hg.

후처리

  1. temperatureThe mixture was warmed until reaction
  2. washwashed with water, hydrochloric acid (2M), water
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customThe filtrate was evaporated to dryness
  6. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-743f0184faad46bdaf8b57fb69cedb4f
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424276

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