Thionyl Chloride → N-(3-chloropropyl)-2-nitro-4-(trifluoromethyl)benzenamine

HRID 354951ノート

反応式

HRID 354951 の反応式
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:6][C:5]=1[NH:14][CH2:15][CH2:16][CH2:17]O)([O-:3])=[O:2].S(Cl)([Cl:21])=O>ClC(Cl)Cl>[Cl:21][CH2:17][CH2:16][CH2:15][NH:14][C:5]1[CH:6]=[CH:7][C:8]([C:10]([F:13])([F:12])[F:11])=[CH:9][C:4]=1[N+:1]([O-:3])=[O:2]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 28475091-Propanol, 3-[[2-nitro-4-(trifluoromethyl)phenyl]amino]-

生成物 1

HCID 20506352N-(3-chloropropyl)-2-nitro-4-(trifluoromethyl)benzenamine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a stirred mixture of 26 parts of 3-{[2-nitro-4-(trifluoromethyl)phenyl]amino}-1-propanol and 150 parts of trichloromethane are added dropwise 40 parts of sulfinyl chloride. Upon completion, stirring is continued overnight at reflux temperature. The reaction mixture is evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5) as eluent. The pure fractions are collected and the eluent is evaporated, yielding N-(3-chloropropyl)-2-nitro-4-(trifluoromethyl)benzenamine as a residue.

後処理

  1. temperatureat reflux temperature
  2. customThe reaction mixture is evaporated
  3. customThe residue is purified by column-chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (95:5) as eluent
  5. customThe pure fractions are collected
  6. customthe eluent is evaporated

出典と根拠

ORDレコード
ord-bde5098fa392448bb2f3cdea25f527a1
出典データセット
uspto-grants-1983_03
特許番号
US04377578

反応ノート

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