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

HRID 21462

反応式

HRID 21462 の反応式
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]

参加物

5

反応物 3

HCID 10906Tert-Butyl nitrite2 回HCID 12232Dimethyl DisulfideHCID 679892-Bromo-5-(trifluoromethyl)benzenamine2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-743f0184faad46bdaf8b57fb69cedb4f
出典データセット
uspto-grants-1995_06
特許番号
US05424276

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